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Ecotoxicology and Public Health

Organic Fluorine as an Indicator of Per- and Polyfluoroalkyl Substances in Dust from Buildings with Healthier versus Conventional Materials
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Environmental Science & Technology

Cite this: Environ. Sci. Technol. 2022, 56, 23, 17090–17099
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https://doi.org/10.1021/acs.est.2c05198
Published November 4, 2022

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Abstract

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Per- and polyfluoroalkyl substances (PFAS) are a class of thousands of persistent, organic fluorinated chemicals added to materials and products mainly to repel stains and water. PFAS have been associated with many adverse human health effects. We aimed to determine whether buildings with “healthier” materials─defined here as reportedly free of all PFAS─exhibit lower PFAS in dust. In addition to analyzing targeted PFAS with available commercial standards, we measured extractable organic fluorine (EOF) as a novel proxy that includes both known and unknown types of PFAS. We measured at least 15 targeted PFAS (n = 24), EOF (n = 24), and total fluorine (TF; n = 14) in dust collected from university common spaces and classrooms, half of which had “healthier” furniture and carpet. We observed lower PFAS contamination in buildings with “healthier” materials: “healthier” rooms had a 66% lower median summed PFAS and a 49% lower Kaplan–Meier estimated mean EOF level in dust in comparison to conventional rooms. The summed targeted PFAS were significantly correlated with EOF but accounted for up to only 9% of EOF, indicating the likely presence of unidentified PFAS. EOF levels explained less than 1% of TF in dust. We emphasize the need to use chemical class-based methods (e.g., EOF) for evaluating class-based solutions and to expand non-PFAS solutions for other building materials.

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Synopsis

There is little research about solutions for PFAS. In this study, buildings with “healthier” materials had lower median levels in dust of known PFAS and organic fluorine, a proxy that includes unknown PFAS.

Introduction

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Per- and polyfluoroalkyl substances (PFAS) are a class of highly fluorinated, anthropogenic chemicals added to products for their surfactant, stain-resistant, and water-resistant properties. (1) To date, over 12,000 different PFAS structures have been identified. (2) Because of concerns about the toxicity and persistence of this class of thousands of chemicals, scientists have called for PFAS to be addressed as a chemical class instead of as one chemical at a time. (3−5) This class-based approach seeks to avoid the common issue of well-known types of PFAS being eliminated in favor of a less-known substitute PFAS with similar concerns for health and the environment. Addressing the prevalent use of PFAS in over 200 different consumer and industrial categories (6) is critical because PFAS have contaminated drinking water and environments on every continent; (7−10) have been detected in the blood of over 98% of Americans; (11) and have been associated with human risk of thyroid disease, stunted development, weakened immune system, high cholesterol, cancer, obesity, and diabetes. (1,12−18)
In recent years, the “healthier” materials movement has advanced alternative building materials that are reported by manufacturers to be free of all types of PFAS, flame retardants, and other chemicals, although these materials are not common yet. One university implemented some of the first interventions to refurnish interiors of certain buildings with “healthier” furniture and carpet that reportedly did not contain any added PFAS (or certain other chemicals), as specified by manufacturers in product purchasing agreements with the university. In our previous study, we scientifically evaluated the effectiveness of the completed interventions at that university. We found that rooms with so-called “healthier” furniture and carpet had 78% significantly lower total levels of 15 measured PFAS in dust compared to rooms with conventional materials, indicating a substantial benefit of “healthier” materials interventions. (19) To our knowledge, no other study has yet been published that evaluates a real-world intervention to reduce exposure to this ubiquitous group of chemicals. In addition, the advancement of class-based analytical methods is needed to fully evaluate the extent of unknown PFAS contamination and the effectiveness of chemical class-based interventions.
Organic fluorine has recently emerged as a novel indicator that encompasses the total content of both known and unknown types of PFAS, unlike traditional targeted analyses that can reliably quantify only a few dozen known PFAS that have commercially available analytical standards. Measurement of total fluorine (TF) is inexpensive, but it is not as reliable of a proxy for PFAS because it includes inorganic fluoride in addition to organic fluorine. By contrast, extractable organic fluorine (EOF) measurements exclude interference from any inorganic fluoride by removal of the inorganic fraction via extraction. (20−23) In the past decade, several studies have measured TF and/or EOF in food packaging, paper, cosmetics, textiles, and firefighter gear. These studies found potentially large quantities of unknown PFAS in the products, with specific measured PFAS usually accounting for up to only about 2% of EOF or TF levels. (22,24−27) Scarce research has been done on EOF or TF in indoor dust, which is a major route of human exposure to PFAS. Because PFAS are noncovalently bound additives, they readily migrate out of materials and accumulate in the dust in buildings. (27−29)
In this study, we investigated the impact of a “healthier” materials intervention in university buildings on levels of targeted PFAS, extractable organic fluorine, and total fluorine in indoor dust. Specifically, our objectives were to (1) compare concentrations of EOF and targeted PFAS in indoor dust samples collected from 12 indoor spaces with “healthier” furnishings versus 12 spaces with conventional furnishings, (2) determine the fraction of EOF and TF that cannot be explained by the known targeted PFAS, and (3) evaluate the strength of correlation between EOF concentrations and TF measurements within a small subset of 14 samples.

Methods

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Study Design

We investigated PFAS and EOF in dust samples collected from 24 rooms in buildings at a university in the United States. These samples were collected in 2019 as part of our previous study of 48 rooms. (19) The study included as many buildings as possible that had undergone a “healthier” carpet and furniture renovation by the university. The “healthier” carpet and furniture were defined here as being reported by manufacturers to be free of all types of PFAS (down to a certain reporting threshold such as 100 ppm), based on product purchasing agreements with the university. The materials were also reported to be free of chemical flame retardants, as investigated in our previous study. “Furniture” referred to furnishings that were generally not fixed within the rooms, except for electronics. We confirmed with the university teams which campus building rooms had undergone the full “healthier” materials intervention and which did not have any intervention on the furniture or carpet (i.e., conventional materials). We selected and categorized rooms as “healthier” or conventional before we collected any dust samples in the selected rooms.
We attempted to choose conventional rooms that were otherwise as similar as possible to “healthier” rooms─among the buildings available to sample─in terms of room characteristics, size, recentness of last renovation, and construction year. The median year of building construction was 1965 for the conventional rooms in this study and 1972 for “healthier” rooms. The median year of last refurnishing was 2016 for conventional rooms (refurnished with conventional materials) and was 2018 for “healthier” rooms (refurnished with “healthier” materials), based on product procurement records or on furniture tags in the rooms. All sampled rooms were carpeted (by study selection criteria), never had stain-repellant coatings applied to carpets (according to the university), and were vacuumed at least two times per week.
For our current substudy, we included 14 common areas and 10 classrooms across 14 unique buildings. This subset of rooms (n = 24) from the parent study (n = 48) was selected randomly to achieve equal numbers of conventional and “healthier” rooms among common areas and classrooms in the parent study with sufficient masses of dust. For secondary analysis of TF in the same dust samples, we analyzed a total of 14 samples (from eight common areas and six classrooms), which were randomly selected for equal numbers across conventional versus “healthier” materials type.

Dust Collection

Each room area was split into thirds, and a separate dust sample was collected within each third of the room for different laboratory analyses (one dust sample for targeted chemicals; one for EOF and TF analysis; and one for cell assays for a different study) (Figure S1). Dust samples were collected by vacuuming floor dust for 10 min into a cellulose extraction thimble secured with a nitrile rubber O-ring inside a crevice tool attached to a vacuum cleaner (Dyson CY18). In this way, the only reused equipment the dust contacted was the crevice tool, which was cleaned with isopropyl alcohol and tap water between uses. After collection, the samples were stored in polypropylene centrifuge tubes in a freezer at −13 °C. Blank thimbles in centrifuge tubes were used as field blanks (n = 4) that were transported to and from each sampling location but never opened. Further details on the sampling protocol are available in our previous contribution. (19)

Sample Extraction and Targeted PFAS Analysis from Previous Study

As part of this study, we included chemical data collected in our previous study of the concentrations of 15 PFAS analytes in the dust samples. (19) These included: perfluorooctanesulfonate (PFOS), perfluorooctanoate (PFOA), perfluorohexanoate (PFHxA), perfluorohexanesulfonate (PFHxS), perfluorooctane sulfonamide (FOSA), perfluoroheptanoate (PFHpA), perfluoropentanoate (PFPeA), perfluorononanoate (PFNA), perfluorobutanesulfonate (PFBS), perfluorodecanesulfonate (PFDS), perfluorobutanoate (PFBA), perfluorodecanoate (PFDA), perfluoroundecanoate (PFUnDA), perfluorododecanoate (PFDoDA), and n-methyl perfluorooctane sulfonamidoacetic acid (N-MeFOSAA).
The 15 targeted PFAS were quantified using high-performance liquid chromatography (HPLC) coupled with electrospray triple quadrupole tandem mass spectrometry (ESI-MS/MS) and monitored by multiple reaction monitoring mode under negative ionization. Prior to extraction, the dust samples were sieved through a 150 μm stainless steel mesh (sample masses: 0.2–0.5 g) and spiked with internal standards (30 ng). They were extracted with 30 mL of methanol, mechanically oscillated for 1 hr, ultrasonicated for 30 min, centrifuged for 10 min (3500g), and transferred into new polypropylene tubes. The extraction was repeated twice with 3 mL of acetonitrile and 3 mL of ethyl acetate, and the extracts were combined and evaporated to 3 mL under nitrogen. The extracts were reconstituted with 200 μL of methanol and filtered through a 0.2 μm nylon filter into glass vials for HPLC analysis. The concentrations of the 15 targeted PFAS were corrected for extraction losses and matrix interferences, because internal standards were added prior to extraction in the methods for the quantification of the 15 targeted PFAS. Additional details are provided in the previous publication. (19)

Sample Extraction for Current Study

For the current study, we analyzed concentrations of EOF in dust samples at the Biogeochemistry of Global Contaminants Laboratory at Harvard University. We analyzed replicate dust samples that had been collected in a different one-third split of each room at the same time as the other dust samples for analysis of 15 targeted PFAS (see diagram in Figure S1). To determine the fraction of EOF explained by measured PFAS, dust samples extracted for EOF analysis included an additional measurement of 37 known PFAS using this laboratory’s targeted analysis method, for direct comparison between measured PFAS and EOF. The targeted analysis method is described in detail in prior publications. (30,31) Since EOF measurements are not recovery-corrected, comparison of PFAS to EOF requires additional analysis of targeted PFAS in which internal standards (ISs) are added after extraction to avoid recovery correction. Concentrations of these 37 nonrecovery-corrected PFAS may be underestimated compared to the 15 PFAS that were measured with ISs added before extraction due to recovery correction based on extraction losses and matrix interferences. Thus, the resulting concentrations from the 37 measured PFAS are used only to calculate the organic fluorine equivalents from measured PFAS in order to evaluate the unknown fraction of EOF. The recovery-corrected concentrations of 15 targeted PFAS measured in the previous study are used to discuss specific PFAS contamination in dust in the buildings and how that varied by intervention type.
For the analysis of EOF (alongside 37 measured PFAS), replicate dust samples (∼200 mg) were left unsieved, extracted with 5 mL of methanol (MeOH) in a 15 mL polypropylene tube, vortexed, and sonicated in a 40 °C water bath for 20 min. Samples were then centrifuged for 5 min at 5000 rpm, and the MeOH extract was decanted to a new tube. This process was repeated two more times, and the extracts were combined. The final 15 mL extract was evaporated to 1 mL using an N-EVAP nitrogen evaporator. The 1 mL sample extracts were loaded onto preconditioned Supelco Envi-carb cartridges (250 mg, 6 mL) and eluted with 3 mL of MeOH. The eluted extract was evaporated to 0.5 mL on the N-EVAP.
To remove inorganic fluoride from the extracts for EOF analysis, (32−34) the 0.5 mL sample extract was diluted with 10 mL of Milli-Q (MQ) water and loaded onto preconditioned Oasis WAX cartridges (150 mg, 30 μm). Following sample loading, cartridges were washed with 20 mL of 0.01% ammonium hydroxide in MQ water and 10 mL of MQ water. Cartridges were dried under vacuum for 30 min and eluted with 4 mL of MeOH and 4 mL of 0.1% ammonium hydroxide in MeOH. Sample extracts were evaporated to dryness, reconstituted in 1 mL of MeOH, and split in half for analysis on the liquid chromatograph-tandem mass spectrometer (LC-MS/MS) for measured PFAS and the combustion ion chromatograph (CIC) for EOF. Isotopically labeled ISs were added to the LC-MS/MS fraction after splitting and combined in 50:50 MQ water–MeOH for analysis.

Analysis of EOF, TF, and PFAS Fluorine Equivalents

Split sample extracts were analyzed at Harvard University for EOF on a Metrohm CIC with combustion unit from Analytik Jena (Jena, Germany), 920 Absorber Module, and 930 Compact IC Flex ion chromatograph from Metrohm (Herisau, Switzerland). Sample extracts (100 μL) were injected into the combustion unit at 1050 °C, and the anions were separated with an ion exchange column (Metrosep A Supp 5-150/4) operated at 30 °C, with sodium carbonate–bicarbonate buffer as eluent and isocratic elution. The fluorine (F–) concentration was measured via ion conductivity.
To determine the fraction of EOF in the extracts explained by organic fluorine equivalents calculated from measured PFAS, 37 targeted analytes were measured using splits of the same sample extracts for EOF determination. Postextraction IS-spiked sample extracts were analyzed on an Agilent (Santa Clara, CA, U.S.A.) 6460 triple quadrupole LC-MS/MS equipped with an Agilent 1290 Infinity Flex Cube online SPE, following previously published methods, with slight modifications. (35) Method detection limits (MDLs) ranged from 0.016 to 4.5 ng/g for the 37 PFAS analyzed (Table S1). Further information on the laboratory methods can be found in the Supporting Information (SI), and mass spectrometry acquisition parameters are detailed in Table S2. The 37 measured PFAS included the same analytes as the previous study plus perfluorotridecanoate (PFTrDA), perfluorotetradecanoate (PFTeDA), perfluoropentanesulfonate (PFPeS), perfluoroheptanesulfonate (PFHpS), perfluorononanesulfonate (PFNS), perfluoro-1-hexanesulfonamide (FHxSA), perfluorodecanesulfonamide (FDSA), perfluoro-1-butanesulfonamide (FBSA), 4:2 fluorotelomer sulfonate (FTSA), 6:2 FTSA, 8:2 FTSA, 10:2 FTSA, 3:3 fluorotelomer carboxylate (FTCA), 5:3 FTCA, 7:3 FTCA, N-ethyl perfluorooctane sulfonamidoacetic acid (N-EtFOSAA), perfluorooctane sulfonamidoacetic acid (FOSAA), N-methyl perfluorooctane sulfonamide (N-MeFOSA), N-ethyl perfluorooctane sulfonamide (N-EtFOSA), N-methyl perfluorooctane sulfonamido ethanol (N-MeFOSE), N-ethyl perfluorooctane sulfonamido ethanol (N-EtFOSE), and dodecafluoro-3H-4,8-dioxanonanoate (ADONA).
TF measurements were carried out using the same Metrohm CIC. Dust material (4.6–10 mg) was weighed directly into a quartz sample boat with quartz insert to keep the sample in place. Quartz sample boats were baked prior to sample combustion to minimize background contamination. The samples were combusted at 1050 °C for approximately 4.5 min. Combustion gases were absorbed in Milli-Q water during the entire length of the combustion process using the 920 Absorber Module, and an aliquot of the absorption solution was injected onto the ion chromatograph. The fluorine (F–) concentrations were measured via ion conductivity.

Quality Assurance and Quality Control

For the primary data on 15 targeted PFAS from the previous study, field blank levels were almost all below the limit of detection (LOD) or well below sample concentrations. More details on the quality assurance/quality control are provided in the previous publication. (19) Information on the quality assurance/quality control of the current analysis of 37 measured PFAS (which were interpreted only in the context of the EOF fraction due to the sample extraction procedure) can be found in the SI.
For EOF analysis, a quartz boat without sample (boat blank) was analyzed twice between each set of duplicate sample injections to determine background fluorine (F–) levels between sample injections. Samples were blank-corrected using the peak areas of the boat blanks run before and after each set of injections. Methanol blanks were run during calibration and after every ten samples to account for any source of contamination from the solvents used in the analysis. Extraction blanks were used to determine the LOD, which was calculated as the average plus three times the standard deviation of duplicate injections of extraction blanks. The extraction LOD was determined to be 514 ng F/mL, and individual sample MDLs were calculated based on the extraction LOD multiplied by each sample’s dilution factor based on sample mass extracted. Sample MDLs ranged from 2177 to 3132 ng F/g. All four field blank samples were less than the MDL. Sample concentrations were determined from the average peak areas of duplicate injections using a nine-point calibration curve (R2 > 0.999) of a custom anion mix in LC-MS grade methanol from 100 to 10,000 μg F/L. Concentrations above the MDL were adjusted for the dilution factor and corrected by subtracting the average field blank concentration. Quality control points were included after every 12 samples and had a variance of <12%. Samples (n = 3) were spiked with inorganic fluoride (IF) to assess removal efficiency with the extraction procedure and were all less than the MDL. The percent recovery (96–105%, n = 3) was calculated from the concentration of organic fluorine measured by the CIC divided by the concentration of organic fluorine measured by the LC-MS/MS using a 1065 μg F/L PFOS spike in extracted MeOH.
For TF analysis, quantification was carried out using a quadratic 13-point calibration curve of single 100 μL injections of a custom anion mix in MQ water ranging from 50 to 80,000 ng F/sample (R2 > 0.999). Quality control calibration checks were included throughout the analysis and had a variance of <6%. The LOD for TF measurements was calculated from the average area obtained from boat blanks run throughout the analysis plus three times the standard deviation of the blanks which resulted in an LOD of 26 ng F/sample. A TF blank of Milli-Q water was tested and yielded a concentration less than the LOD. Dust sample concentrations were blank-corrected using the field blank (cellulose extraction thimble used to collect dust) due to detectable levels of F– in the field blanks that accounted for up to 3% of the fluorine concentration measured in the dust samples. A 15,030 ng F/sample sodium fluoride spike in Milli-Q water was included to assess combustion efficiency and recovery (109% recovery). TF concentrations were converted to ng F/g based on the sample mass combusted.

Statistical Analysis

All EOF, TF, and PFAS concentrations were blank-corrected by subtracting the average value of the field blanks. We calculated the sum of targeted PFAS levels by summing the individual concentrations of the analytes, where values less than MDL were treated as the MDL divided by the square root of two.
For statistical analyses of EOF, we substituted concentrations of EOF less than the MDL with the MDL divided by the square root of two. However, we also performed alternative statistical analyses of EOF using nonparametric reverse Kaplan–Meier (KM) estimation, which is often preferred over simple substitution methods because it accounts for left censored data with multiple different─and comparatively high─detection limits for EOF in the samples, which is less of an issue in targeted PFAS analysis. The lowest observed EOF concentrations were not censored nondetects, so no correction method was needed for KM estimation, and 33% of the EOF data were censored. The KM estimation does not make distributional assumptions. (36,37) This approach was not needed for the PFAS concentrations due to lower, more sensitive detection limits.
Significant differences in the levels of PFAS and EOF between conventional versus “healthier” rooms were assessed using nonparametric Wilcoxon rank sum tests or using Peto–Prentice tests for Kaplan–Meier estimates. Correlations were calculated as nonparametric Spearman coefficients. Statistical significance was evaluated at α = 0.05 with suggestive evidence at α = 0.10.
To investigate the fraction of EOF or TF not accounted for by measured PFAS, we converted the levels of each PFAS to organic fluorine equivalents using the following equation (25) and then summed them for each sample:
CF=CPFASnF·AWFMWPFAS
where CF is the calculated fluorine concentration (ng F/g) in the dust from that PFAS, CPFAS the concentration (ng/g) of each PFAS in the dust, nF the number of fluorine atoms on each PFAS, AWF the atomic weight of fluorine (18.998 g/mol), and MWPFAS the molecular weight of each PFAS (g/mol). For each sample, we calculated the sum of the organic fluorine equivalents for all PFAS and divided this by the actual measured EOF or TF concentration as an indicator of the percent of EOF or TF accounted for by these targeted analytes. All analyses were conducted in R (version 4.1.2).

Results

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Targeted PFAS

In the samples of dust from 24 common areas or classrooms at a university, the summed concentrations of targeted PFAS were significantly lower in the rooms with “healthier” materials specified to be free of all PFAS in comparison to the rooms with conventional materials. Specifically, the median sum of 15 targeted PFAS in the dust samples was 66% lower in the 12 rooms with “healthier” materials compared to the 12 conventional rooms. The differences were statistically significant with p = 0.0001. The median [range] was 403 [226–1750] ng/g for conventional rooms and 136 [19.5–422] ng/g for “healthier” rooms (Table 1).
Table 1. Medians, Ranges, and Kaplan–Meier (KM) Estimated Means for Concentrations of Total Fluorine (TF), Extractable Organic Fluorine (EOF), and the Sum of 15 Targeted PFAS in up to 24 Samples of Indoor Dust from University Spaces with Either Conventional Materials or “Healthier” Materials Reported to Be Free of All PFASa
   all roomsconventional rooms“healthier” rooms
parameterunitsnmedianrangemedianKM meanrangemedianKM meanrange
total fluorine (organic + inorganic)ng F/g142190000[<MDL–17800000]2330000 [<MDL–17800000]1810000 [657000–13800000]
extractable organic fluorineng F/g241830[<MDL–17600]20503390[<MDL–17600]17701720[<MDL–4730]
sum of 15 targeted PFAS (recovery-corrected)ng/g24274[19.5–1750]403 [226–1750]136 [19.5–422]
a

Reverse Kaplan–Meier (KM) estimation was used as an alternative, nonparametric approach for summarizing mean EOF concentrations because of the multiple, relatively high detection limits in these left-censored data; by contrast, the median and range of EOF levels were based on simple nondetect substitution. Sample sizes were split equally between conventional rooms and “healthier” rooms (n = 12 of each category for EOF and PFAS measurements; n = 7 each for TF measurements).

Organic Fluorine

Across all 24 conventional and “healthier” rooms, there was a median 1,830 ng F/g of extractable organic fluorine and maximum 17,600 ng F/g (Table 1). Levels of EOF were above the method detection limit in 67% of dust samples (16 of 24). Samples with levels less than the MDL were collected from 5 “healthier” rooms and 3 conventional rooms.
The summarized concentrations of extractable organic fluorine were lower in dust from the rooms with “healthier” materials compared to rooms with conventional materials (Figure 1). The median EOF was 14% lower in “healthier” rooms (1,770 ng F/g [range: <MDL–4,730 ng F/g]) than in conventional rooms (2,050 ng F/g [<MDL–17,600 ng F/g]; p = 0.083) (Table 1) with suggestive evidence (defined as p ≤ 0.1). Based on reverse Kaplan–Meier estimation, which better accounts for the relatively high detection limits compared to targeted PFAS analysis, the mean EOF levels in dust were 49% lower in rooms with “healthier” materials (1,720 ng F/g) compared to rooms with conventional materials (3,390 ng F/g) (Table 1). Differences between EOF concentrations in “healthier” rooms and conventional rooms were more pronounced using reverse Kaplan–Meier mean estimation, although this difference did not reach statistical significance due to small sample numbers (suggestive evidence at p = 0.1). The 95% confidence intervals (CIs) for the KM means of EOF were 1,720 ng F/g (95% CI: 1,020–2,420 ng F/g) for “healthier” rooms and 3,390 ng F/g (727–6,050 ng F/g) for conventional rooms.

Figure 1

Figure 1. Concentrations of the sum of 15 targeted PFAS (ng/g) (left panel) and extractable organic fluorine (EOF) (ng F/g) (right panel) in 24 dust samples from rooms with conventional or “healthier” building materials.

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The calculated organic fluorine equivalents based on 37 measured PFAS from the EOF extraction also had a 53% lower median concentration in rooms with “healthier” materials (25.4 ng F/g [range: 15.0–51.5 ng F/g]) compared to conventional materials (54.5 ng F/g [24.5–597 ng F/g]), and this difference was statistically significant (p = 0.0045) (Table 1). These 37 measured PFAS were not recovery-corrected during laboratory analysis in this study (unlike the 15 targeted PFAS from our previous analysis) in order to have direct comparison to EOF levels, as described in detail in Methods.
Figure 2 demonstrates the substantial difference in magnitudes between levels of measured EOF and organic fluorine equivalents calculated from the 37 measured PFAS, even while both indicators had medians that were lower in “healthier” rooms compared to conventional rooms (Figure 2). Across all samples, the EOF concentrations had a median of 1,830 and maximum of 17,600 ng F/g, whereas the calculated concentrations of organic fluorine equivalents based on the measured PFAS had a median of 39.5 and maximum of 597 ng F/g (Table 1). The measured PFAS only accounted for between 1.0 and 9.2% (median 2.6%) of the EOF concentrations among the 16 samples with detectable EOF. There were significant positive correlations between the EOF levels and the organic fluorine equivalents of 37 measured PFAS (Spearman r = 0.47, p = 0.020) and the sum of recovery-corrected concentrations of 15 targeted PFAS from the previous study (r = 0.43, p = 0.034).

Figure 2

Figure 2. Median concentrations (ng F/g) of total fluorine, extractable organic fluorine (EOF), and calculated organic fluorine equivalents based on measured PFAS in dust samples from n = 24 rooms with conventional or “healthier” materials.

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Total Fluorine

All but one sample had levels of total fluorine above detection limits. The concentrations of TF, which includes both organic and inorganic fluorine, were orders of magnitude higher than the measured concentrations of extractable organic fluorine (Table 1). In fact, the percent of TF explained by EOF was <1% in all samples with detectable levels of both TF and EOF (range: 0.014–0.61%). Similarly, among the samples with measured and detectable levels of TF, only up to 0.021% (min: 0.00028%) of TF was accounted for by the organic fluorine equivalents calculated from the 37 measured PFAS. Although TF was only moderately correlated with EOF (Spearman r = 0.45, p = 0.11) and had a small sample size (n = 14), we did observe a nonsignificant 22% lower median concentration of TF in dust from the rooms with “healthier” materials (1,810,000 ng F/g [range: 657,000–13,800,000 ng F/g]) compared to conventional rooms (2,330,000 ng F/g [<MDL–17,800,000 ng F/g]) (p = 0.53) (Figure 2 and Table 1).

Discussion

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In a novel intervention, buildings with reportedly “healthier” furniture and carpet had lower summarized levels of both known PFAS and organic fluorine in dust compared to buildings with conventional materials at a university. The “healthier” materials in this study were specified by manufacturers (in agreements with the university) to be free of the entire chemical class of PFAS. While our laboratory analysis quantified only up to 37 specific PFAS in the dust for comparison to EOF, our measurement of EOF acts as a novel proxy that may encompass the total fluorinated content of thousands of variants of PFAS that are often substituted for each other in products. (2,23) Thus, this study was able to demonstrate suggestive evidence that the rooms with “healthier” materials did have nearly half the mean dust levels of EOF (based on KM estimation), in addition to significantly lower levels of the small subset of widely known PFAS. Even without being able to intervene on building structural materials or the consumer products that people bring into buildings, the interior furnishing renovations were associated with lower PFAS contamination. The expected reduction in PFAS and EOF concentrations in dust in buildings with “healthier” carpet and furniture is supported by previous evidence of high levels of PFAS and fluorine on carpets and upholstery at a U.S. university campus. (27) Our study highlights the importance of employing chemical class-based analytical methods for the evaluation of chemical class-based “healthier” material solutions. Because of the prevalent and repeated substitution of less-known PFAS for well-known PFAS over time, (3) we must motivate long-term solutions that are shown to be effective at eliminating the whole PFAS class.
There were some nuances in the difference in reduction level between EOF and targeted PFAS for the conventional versus “healthier” rooms. The reduction in the total levels of targeted PFAS in dust had strong statistical significance while the reduction in EOF had suggestive evidence. This may be influenced by a combination of several possible reasons. First and perhaps most important, our small sample size for this analysis (n = 24) did limit the statistical power of our significance tests. Second, EOF measurements are well-established to have limitations of lower sensitivity (higher detection limits) compared to targeted PFAS analysis, (23) so statistical analyses have to make stronger assumptions when substituting nondetect EOF values. Third, it is possible that any other organic fluorinated chemicals captured by EOF (e.g., some refrigerants, pharmaceuticals, or pesticides), (38,39) even if at low levels and similar between conventional and “healthier” rooms, could slightly dilute the observable reductions in PFAS. Fourth, a large prevalence of unknown PFAS (which would be picked up by EOF but not targeted PFAS analysis) could be brought in from many other building material or product categories besides interior furniture and carpet. (6) The “healthier” rooms may have had slightly newer ages of other building materials that could not be intervened on and thus potentially more unknown, emerging PFAS substitutes used in those additional sources. The median year of building construction for the conventional rooms was 1965 [1925–2016] compared to 1972 [1966–2018] for “healthier” rooms. Fifth, the reported elimination of all PFAS, including unknown types, by manufacturers was not verified in these early (often custom-designed) “healthier” materials and may not have applied to trace concentrations of PFAS (e.g., <100 ppm) or unintentional contamination in the supply chain and production process. Nonetheless, these early “healthier” materials interventions on carpet and furniture did provide notable benefits for reducing content of these chemicals in buildings. Our results build scientific evidence for an expansion of chemical class-based solutions to more product categories that could further reduce PFAS contamination in buildings (e.g., structural building materials, flooring, sealants, adhesives, paints, coatings, electronics, glass, and pipes). (6) To grow the “healthier” materials movement, there needs to be sufficient guidance for manufacturers and capital project teams on a definition of PFAS that is clear and nonambiguous (40) and that ensures the elimination of PFAS variants that have not been formally identified yet.
The relatively low fraction (up to 9%) of extractable organic fluorine accounted for by 37 PFAS simultaneously measured in the dust indicates a potentially large contribution of other unidentified PFAS and demonstrates the importance of addressing PFAS as a class. The PFAS measured in this study did not include some known types of PFAS such as fluorotelomer alcohols (FTOHs) and polyfluoroalkyl phosphoric acid diesters (diPAPs), which are commonly found in indoor dust. (41,42) However, even if we estimate the potential fluorine contribution of these chemicals based on the geometric means of the commonly detected 8:2 and 10:2 FTOHs in dust from office buildings in Boston (most similar to our study) (43) and the median of the frequently detected 6:2 diPAP in dust from homes in North Carolina, (42) over half of the EOF levels in our study would still be left unaccounted for in all but two of our samples. Other non-PFAS types of organic fluorinated compounds (including refrigerants, pharmaceuticals, or pesticides) (38,39) could have been tracked into the buildings at low levels but are also unlikely to constitute a major proportion of EOF or to explain away the intervention results; any contamination would have been similar between the conventional and “healthier” rooms within the same university, and we did discern reductions in EOF with the “PFAS-free” materials intervention.
The low explained fraction of EOF aligns with most previous studies of fluorine in other types of samples. In one study, 44 measured PFAS (including diPAPs) accounted for up to only 0.3% of the EOF levels in nine samples of disposable food packaging. (22) In another study, 39 measured PFAS (including diPAPs) explained less than 1.3% of EOF in 28 of the cosmetics samples (up to 28% in three other samples with the highest levels). (25) To our knowledge, there is only one other online report (by an environmental institute) of EOF levels in indoor dust. (44) The authors found that 20 measured anionic PFAS (including FTOHs) explained between 10% and over 100% of the EOF levels measured in duplicates of the dust samples. However, in this study they compared recovery-corrected PFAS concentrations from the targeted analysis to nonrecovery-corrected (likely underestimated) EOF concentrations. Since different extraction and cleanup methodologies with internal standard addition were used for these two analyses (as the authors acknowledge), these PFAS and EOF results should not be directly compared. (44) This prior result is not comparable to the current study because we directly compared EOF and PFAS measurements using equivalent methods and because we measured orders of magnitude higher EOF and summed PFAS concentrations in building dust in our study (max EOF: 17,600 ng F/g; max PFAS: 1,750 ng/g) compared to their study (max EOF: 96 ng F/g; max PFAS: 79 ng/g).
A very low percent of total fluorine (less than 1%) was accounted for by extractable organic fluorine levels in our dust samples, suggesting that EOF is a more relevant proxy for total PFAS in dust matrices. Previous studies also observed low explained fractions of TF by EOF, although with consumer products. For example, EOF accounted for up to 5.5% of TF levels in disposable food packaging samples (22) and an average of 9% of TF levels in cosmetic samples. (25) The orders of magnitude difference between EOF and TF in our dust samples is likely influenced by inorganic fluoride from natural soil in the dust samples. (45) Because of the potentially large contribution to TF from inorganic fluoride, measurements of EOF in dust are more specific and useful as proxies for total PFAS content. Future studies should advance methods to directly measure levels of inorganic fluoride in indoor dust and other solid matrices to determine how much of the TF is explained by inorganic fluoride as opposed to unextractable PFAS or other fluorinated chemicals. (25) In any future research, the choice of methods should consider the sample matrix type (e.g., dust, water, soil, consumer products), which can have varying interference from inorganic fluoride or fluorinated pharmaceuticals/pesticides; the feasibility of sample treatment (e.g., nondestructive direct analysis versus extraction); the need for low limits of detection; the preference of either surface fluorine measurements or average full-sample measurements; and any need for high-throughput screening of many samples. (23,46) An ideal workflow recently described by Koch et al. (2020) suggests analysis of organic fluorine in samples followed by the measurement of targeted PFAS in at least a subset of samples; if unquantifiable/unknown organic fluorine is substantial, it can then be identified via other approaches (e.g., nontargeted analysis, suspect screening, or total oxidizable precursor [TOP] assays). (46)
There were several strengths of our study. This study, along with our previous publication about the same buildings, were the first to evaluate the benefits of a real-world intervention to reduce exposure to the concerning, ubiquitous group of PFAS at the source. Furthermore, our study focused on chemical class-based solutions that are intended to prevent common issues with regrettable substitution of one type of PFAS for another. In addition, to our knowledge this is the first research study of extractable organic fluorine in indoor dust samples, which represent real-world mixtures that are a major route of human exposure, and EOF measurements have the advantage over total fluorine measurements of excluding irrelevant contributions from inorganic fluoride. The pairing of EOF analysis with novel “healthier” materials interventions enabled us to quantify the potential reduction in PFAS as an entire class in dust due to “healthier” furniture choices. In addition, in comparing rooms that had similar characteristics except for the use of conventional versus “healthier” materials, any other non-PFAS organic fluorinated chemicals interfering with EOF levels in the dust would have been similar between the two room categories. In that way, we were able to pinpoint differences in EOF that were mostly driven by PFAS. Furthermore, because we collected multiple dust samples within different splits of each room, we were able to conduct several analyses on the dust samples, including TF, EOF, targeted PFAS (recovery-corrected), and nonrecovery-corrected PFAS for comparison to the fluorine measurements.
Limitations of this study included the small sample size (n = 24), especially for the subset analyzed for total fluorine (n = 14), which limited the statistical power of our analyses. The detection limits for EOF in the dust samples were relatively high, which is a well-established limitation across sample matrices due to the lower sensitivity compared to targeted analysis. (23) As a result, summary statistics based on EOF levels where nondetects were substituted with MDL ÷ √2 may have overestimated the levels in especially “healthier” rooms. Another limitation is the possibility that hair could have been captured in the dust extracts analyzed for EOF, but the EOF and the PFAS measured alongside EOF were still significantly correlated with the PFAS measured in our previous study in dust duplicates that had been sieved down to 150 μm to exclude hair and any other materials. (19) Furthermore, our targeted PFAS analytes did not include all common types of PFAS in indoor dust, such as diPAPs and FTOHs, as discussed previously. EOF measurements would serve as much simpler and more comprehensive proxies of total PFAS content than attempting to measure as many targeted PFAS as feasible. In terms of study design, we attempted to sample conventional rooms that were refurnished as recently as possible (with conventional materials), but they still had a slightly older median year of last refurnishing compared to “healthier” rooms. However, these spaces are all vacuumed very frequently by professional maintenance, so any old dust is minimized; before our sampling, we asked that rooms be left unvacuumed for 2–3 days to ensure there was sufficient recent dust buildup in all the sampled rooms. Finally, we could not analyze the “healthier” materials themselves to verify the absence of PFAS.
In conclusion, compared to university classrooms and common spaces with conventional materials, the equivalent rooms with “healthier” PFAS-free furniture and carpet had lower median dust concentrations of both known PFAS and extractable organic fluorine, which is a proxy that accounts for the total content of all known and unknown types of PFAS. Thus, the “healthier” materials solutions were beneficial for reducing the accumulation of PFAS inside buildings. The organic fluorine measurements demonstrated the importance of chemical class-based analytical methods for investigating the effectiveness of class-based materials solutions. Such “healthier” furniture and carpet materials free of all types of PFAS still need to become more widely available options (or preferably, defaults) and should provide fully disclosed, third-party-verified chemical ingredient lists from manufacturers. Furthermore, “healthier” alternatives need to be developed for other categories of products to further reduce PFAS exposure in buildings.

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The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acs.est.2c05198.

  • Detailed description and tables of methods for analysis of 37 measured PFAS following the EOF extraction protocol (PDF)

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Acknowledgments

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We would like to thank Heather Henriksen for her support of this study. We would like to acknowledge Dr. Kannan Kurunthachalam and Dr. Hong Kai Zhu for their prior collaboration on the measurement of targeted chemicals in the dust samples. We also thank Dr. Aaron Specht for his help with dust analysis. This research was made possible by NIEHS Grant T32 ES007069, NIOSH Grant T42 OH008416, NIH Grant P30ES000002, and the Harvard Campus Sustainability Innovation Fund. Its contents are solely the responsibility of the authors and do not necessarily represent the official views of the funders.

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    Calafat, Antonia M.; Wong, Lee-Yang; Kuklenyik, Zsuzsanna; Reidy, John A.; Needham, Larry L.
    Environmental Health Perspectives (2007), 115 (11), 1596-1602CODEN: EVHPAZ; ISSN:0091-6765. (U. S. Department of Health and Human Services, Public Health Services)
    Polyfluoroalkyl chems. (PFCs) have been used since the 1950s in numerous com. applications. Exposure of the general U.S. population to PFCs is widespread. Since 2002, the manufg. practices for PFCs in the United States have changed considerably. We aimed to assess exposure to perfluorooctane sulfonic acid (PFOS), perfluorooctanoic acid (PFOA), perfluorohexane sulfonic acid (PFHxS), perfluorononanoic acid (PFNA), and eight other PFCs in a representative 2003-2004 sample of the general U.S. population ≥ 12 years of age and to det. whether serum concns. have changed since the 1999-2000 National Health and Nutrition Examn. Survey (NHANES). By using automated solid-phase extn. coupled to isotope diln.-high-performance liq. chromatog.-tandem mass spectrometry, we analyzed 2094 serum samples collected from NHANES 2003-2004 participants. We detected PFOS, PFOA, PFHxS, and PFNA in >98% of the samples. Concns. differed by race/ethnicity and sex. Geometric mean concns. were significantly lower (approx. 32% for PFOS, 25% for PFOA, 10% for PFHxS) and higher (100%, PFNA) than the concns. reported in NHANES 1999-2000 (p < 0.001). In the general U.S. population in 2003-2004, PFOS, PFOA, PFHxS, and PFNA serum concns. were measurable in each demog. population group studied. Geometric mean concns. of PFOS, PFOA, and PFHxS in 2003-2004 were lower than in 1999-2000. The apparent redns. in concns. of PFOS, PFOA, and PFHxS most likely are related to discontinuation in 2002 of industrial prodn. by electrochem. fluorination of PFOS and related perfluorooctanesulfonyl fluoride compds.
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    Fenton, S. E.; Ducatman, A.; Boobis, A.; DeWitt, J. C.; Lau, C.; Ng, C.; Smith, J. S.; Roberts, S. M. Per- and Polyfluoroalkyl Substance Toxicity and Human Health Review: Current State of Knowledge and Strategies for Informing Future Research. Environ. Toxicol. Chem. 2021, 40 (3), 606– 630,  DOI: 10.1002/etc.4890
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    12
    Per- and Polyfluoroalkyl Substance Toxicity and Human Health Review: Current State of Knowledge and Strategies for Informing Future Research
    Fenton, Suzanne E.; Ducatman, Alan; Boobis, Alan; DeWitt, Jamie C.; Lau, Christopher; Ng, Carla; Smith, James S.; Roberts, Stephen M.
    Environmental Toxicology and Chemistry (2021), 40 (3), 606-630CODEN: ETOCDK; ISSN:0730-7268. (Wiley-Blackwell)
    Reports of environmental and human health impacts of per- and polyfluoroalkyl substances (PFAS) have greatly increased in the peer-reviewed literature. The goals of the present review are to assess the state of the science regarding toxicol. effects of PFAS and to develop strategies for advancing knowledge on the health effects of this large family of chems. Currently, much of the toxicity data available for PFAS are for a handful of chems., primarily legacy PFAS such as perfluorooctanoic acid and perfluorooctane sulfonate. Epidemiol. studies have revealed assocns. between exposure to specific PFAS and a variety of health effects, including altered immune and thyroid function, liver disease, lipid and insulin dysregulation, kidney disease, adverse reproductive and developmental outcomes, and cancer. Concordance with exptl. animal data exists for many of these effects. However, information on modes of action and adverse outcome pathways must be expanded, and profound differences in PFAS toxicokinetic properties must be considered in understanding differences in responses between the sexes and among species and life stages. With many health effects noted for a relatively few example compds. and hundreds of other PFAS in commerce lacking toxicity data, more contemporary and high-throughput approaches such as read-across, mol. dynamics, and protein modeling are proposed to accelerate the development of toxicity information on emerging and legacy PFAS, individually and as mixts. In addn., an appropriate degree of precaution, given what is already known from the PFAS examples noted, may be needed to protect human health. Environ Toxicol Chem 2020;00:1-25. 2020 SETAC.
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    Rappazzo, K. M.; Coffman, E.; Hines, E. P. Exposure to Perfluorinated Alkyl Substances and Health Outcomes in Children: A Systematic Review of the Epidemiologic Literature. Int. J. Environ. Res. Public Health 2017, 14 (7), 691,  DOI: 10.3390/ijerph14070691
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    13
    Exposure to perfluorinated alkyl substances and health outcomes in children: a systematic review of the epidemiologic literature
    Rappazzo, Kristen M.; Coffman, Evan; Hines, Erin P.
    International Journal of Environmental Research and Public Health (2017), 14 (7), 691/1-691/22CODEN: IJERGQ; ISSN:1660-4601. (MDPI AG)
    Perfluoroalkyl substances (PFAS), chems. used to make products stain and stick resistant, have been linked to health effects in adults and adverse birth outcomes. A growing body of literature also addresses health effects in children exposed to PFAS. This review summarizes the epidemiol. evidence for relationships between prenatal and/or childhood exposure to PFAS and health outcomes in children as well as to provide a risk of bias anal. of the literature. A systematic review was performed by searching PubMed for studies on PFAS and child health outcomes. We identified 64 studies for inclusion and performed risk of bias anal. on those studies. We detd. that risk of bias across studies was low to moderate. Six categories of health outcomes emerged. These were: immunity/infection/asthma, cardio-metabolic, neurodevelopmental/attention, thyroid, renal, and puberty onset. While there are a limited no. of studies for any one particular health outcome, there is evidence for pos. assocns. between PFAS and dyslipidemia, immunity (including vaccine response and asthma), renal function, and age at menarche. One finding of note is that while PFASs are mixts. of multiple compds. few studies examine them as such, therefore the role of these compds. as complex mixts. remains largely unknown.
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    Xiao, C.; Grandjean, P.; Valvi, D.; Nielsen, F.; Jensen, T. K.; Weihe, P.; Oulhote, Y. Associations of Exposure to Perfluoroalkyl Substances with Thyroid Hormone Concentrations and Birth Size. J. Clin. Endocrinol. Metab 2019, 735,  DOI: 10.1210/clinem/dgz147
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  15. 15
    Lin, P.-I. D.; Cardenas, A.; Hauser, R.; Gold, D. R.; Kleinman, K. P.; Hivert, M.-F.; Fleisch, A. F.; Calafat, A. M.; Webster, T. F.; Horton, E. S.; Oken, E. Per- and Polyfluoroalkyl Substances and Blood Lipid Levels in Pre-Diabetic Adults-Longitudinal Analysis of the Diabetes Prevention Program Outcomes Study. Environ. Int. 2019, 129, 343– 353,  DOI: 10.1016/j.envint.2019.05.027
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    15
    Per- and polyfluoroalkyl substances and blood lipid levels in pre-diabetic adults-longitudinal analysis of the diabetes prevention program outcomes study
    Lin, Pi-I. D.; Cardenas, Andres; Hauser, Russ; Gold, Diane R.; Kleinman, Ken P.; Hivert, Marie-France; Fleisch, Abby F.; Calafat, Antonia M.; Webster, Thomas F.; Horton, Edward S.; Oken, Emily
    Environment International (2019), 129 (), 343-353CODEN: ENVIDV; ISSN:0160-4120. (Elsevier Ltd.)
    We examd. the relationship of baseline plasma PFAS concns. with repeated measures of blood lipids. We included 888 prediabetic adults from the Diabetes Prevention Program (DPP) and DPP Outcomes Study, who had measurements of 6 plasma PFAS concns. at baseline (1996-1999) and repeated measures of blood lipids over 15 years of follow-up, and were initially randomized to placebo or a lifestyle intervention. Participants (65.9% female, 57.0% White, 65.9% aged 40-59 years) had comparable PFAS concns. [e.g., median (IQR) perfluorooctanoic acid (PFOA) 4.9 ng/mL (3.2)] with the general U. S. population in 1999-2000. We obsd. higher total cholesterol at baseline per doubling of PFOA (β: 6.1 mg/dL, 95% CI: 3.1, 9.04), perfluorohexane sulfonic acid (PFHxS, β: 2.2 mg/dL, 95% CI: 0.2, 4.3), and perfluorononanoic acid (PFNA, β: 2.9 mg/dL, 95% CI: 0.7, 5.0). Prospectively, baseline concns. of several PFASs, including PFOA, PFOS, PFHxS and PFNA, predicted higher risks of incident hypercholesterolemia and hypertriglyceridemia, but only in the placebo group and not the lifestyle intervention group. For example, participants in the placebo group with PFOA concn. > median (4.9 ng/mL) were almost twice as likely (HR: 1.90, 95% CI: 1.25, 2.88) to develop hypertriglyceridemia compared to those ≤median. Findings suggest adverse effects of some PFASs on lipid profiles in prediabetic adults. However, the detrimental effect was attenuated with a lifestyle intervention.
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    Liew, Z.; Goudarzi, H.; Oulhote, Y. Developmental Exposures to Perfluoroalkyl Substances (PFASs): An Update of Associated Health Outcomes. Curr. Environ. Heal. reports 2018, 5 (1), 1– 19,  DOI: 10.1007/s40572-018-0173-4
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    Developmental Exposures to Perfluoroalkyl Substances (PFASs): An Update of Associated Health Outcomes
    Liew, Zeyan; Goudarzi, Houman; Oulhote, Youssef
    Current Environmental Health Reports (2018), 5 (1), 1-19CODEN: CEHRB3; ISSN:2196-5412. (Springer International Publishing AG)
    Purpose of Review: We reviewed and summarized the epidemiol. evidence for the influence that pre- and postnatal exposures to perfluoroalkyl substances (PFASs) may have on health outcomes in offspring, with a particular focus on birth outcomes and postnatal growth, immunomodulatory effects and neurodevelopment. Recent Findings: PFASs are persistent org. pollutants that have been widely produced and used in a range of com. products since the 1950s. Human exposures to PFASs are nearly ubiquitous globally, but studies that addressed potential health effects of PFASs have only begun to accumulate in recent years. Animal studies suggest adverse effects resulting from developmental encompasses prenatal exposures to PFASs. In humans, the developing fetus is exposed to PFASs via active or passive placenta transfer, while newborns might be exposed via breastfeeding or PFAS in the home environment. Summary: Overall, epidemiol. findings are consistent and suggest possible assocns. with fetal and postnatal growth and immune function, while the findings on neurodevelopmental endpoints to date are rather inconclusive. Methodol. challenges and future directions for PFASs-focused research are discussed.
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    Barry, V.; Winquist, A.; Steenland, K. Perfluorooctanoic Acid (PFOA) Exposures and Incident Cancers among Adults Living near a Chemical Plant. Environ. Health Perspect 2013, 121 (11–12), 1313– 1318,  DOI: 10.1289/ehp.1306615
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    Perfluorooctanoic acid (PFOA) exposures and incident cancers among adults living near a chemical plant
    Barry Vaughn; Winquist Andrea; Steenland Kyle
    Environmental health perspectives (2013), 121 (11-12), 1313-8 ISSN:.
    BACKGROUND: Perfluorooctanoic acid (PFOA) is a synthetic chemical ubiquitous in the serum of U.S. residents. It causes liver, testicular, and pancreatic tumors in rats. Human studies are sparse. OBJECTIVE: We examined cancer incidence in Mid-Ohio Valley residents exposed to PFOA in drinking water due to chemical plant emissions. METHODS: The cohort consisted of adult community residents who resided in contaminated water districts or worked at a local chemical plant. Most participated in a 2005-2006 baseline survey in which serum PFOA was measured. We interviewed the cohort in 2008-2011 to obtain further medical history. Retrospective yearly PFOA serum concentrations were estimated for each participant from 1952 through 2011. Self-reported cancers were validated through medical records and cancer registry review. We estimated the association between cancer and cumulative PFOA serum concentration using proportional hazards models. RESULTS: Participants (n = 32,254) reported 2,507 validated cancers (21 different cancer types). Estimated cumulative serum PFOA concentrations were positively associated with kidney and testicular cancer [hazard ratio (HR) = 1.10; 95% CI: 0.98, 1.24 and HR = 1.34; 95% CI: 1.00, 1.79, respectively, for 1-unit increases in ln-transformed serum PFOA]. Categorical analyses also indicated positive trends with increasing exposures for both cancers: for kidney cancer HRs for increasing exposure quartiles were 1.0, 1.23, 1.48, and 1.58 (linear trend test p = 0.18) and for testicular cancer, HRs were 1.0, 1.04, 1.91, 3.17 (linear trend test p = 0.04). CONCLUSIONS: PFOA exposure was associated with kidney and testicular cancer in this population. Because this is largely a survivor cohort, findings must be interpreted with caution, especially for highly fatal cancers such as pancreatic and lung cancer.
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    Stanifer, J. W.; Stapleton, H. M.; Souma, T.; Wittmer, A.; Zhao, X.; Boulware, L. E. Perfluorinated Chemicals as Emerging Environmental Threats to Kidney Health: A Scoping Review. Clin. J. Am. Soc. Nephrol 2018, 13 (10), 1479– 1492,  DOI: 10.2215/CJN.04670418
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    Perfluorinated chemicals as emerging environmental threats to kidney health: a scoping review
    Stanifer, John W.; Stapleton, Heather M.; Souma, Tomokazu; Wittmer, Ashley; Zhao, Xinlu; Boulware, L. Ebony
    Clinical Journal of the American Society of Nephrology (2018), 13 (10), 1479-1492CODEN: CJASC7; ISSN:1555-9041. (American Society of Nephrology)
    Background and objectives Per- and polyfluoroalkyl substances (PFASs) are a large group of manufd. nonbiodegradable compds. Despite increasing awareness as global pollutants, the impact of PFAS exposure on human health is not well understood, and there are growing concerns for adverse effects on kidney function. Therefore, we conducted a scoping review to summarize and identify gaps in the understanding between PFAS exposure and kidney health. Design, setting, participants, & measurements We systematically searched PubMed, EMBASE, EBSCO Global Health, World Health Organization Global Index, and Web of Science for studies published from 1990 to 2018. We included studies on the epidemiol., pharmacokinetics, or toxicol. of PFAS exposure and kidney-related health, including clin., histol., mol., and metabolic outcomes related to kidney disease, or outcomes related to the pharmacokinetic role of the kidneys. Results We identified 74 studies, including 21 epidemiol., 13 pharmacokinetic, and 40 toxicol. studies. Three population-based epidemiol. studies demonstrated assocns. between PFAS exposure and lower kidney function. Along with toxicol. studies (n = 10) showing tubular histol. and cellular changes from PFAS exposure, pharmacokinetic studies (n=5) demonstrated the kidneys were major routes of elimination, with active proximal tubule transport.
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    Young, A. S.; Hauser, R.; James-Todd, T. M.; Coull, B. A.; Zhu, H.; Kannan, K.; Specht, A. J.; Bliss, M. S.; Allen, J. G. Impact of “Healthier” Materials Interventions on Dust Concentrations of per- and Polyfluoroalkyl Substances, Polybrominated Diphenyl Ethers, and Organophosphate Esters. Environ. Int. 2021, 150, 106151,  DOI: 10.1016/j.envint.2020.106151
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    Impact of "healthier" materials interventions on dust concentrations of per- and polyfluoroalkyl substances, polybrominated diphenyl ethers, and organophosphate esters
    Young, Anna S.; Hauser, Russ; James-Todd, Tamarra M.; Coull, Brent A.; Zhu, Hongkai; Kannan, Kurunthachalam; Specht, Aaron J.; Bliss, Maya S.; Allen, Joseph G.
    Environment International (2021), 150 (), 106151CODEN: ENVIDV; ISSN:0160-4120. (Elsevier Ltd.)
    Per- and polyfluoroalkyl substances (PFAS), polybrominated di-Ph ethers (PBDEs), and organophosphate esters (OPEs) are found in building materials and assocd. with thyroid disease, infertility, and impaired development. We measured 15 PFAS, 8 PBDEs, and 19 OPEs in dust from offices, common areas, and class rooms having undergone either no intervention (conventional rooms in older buildings meeting strict fire codes; n = 12), full "healthier" materials interventions (rooms with "healthier" materials in buildings constructed more recently or gut-renovated; n = 7), or partial interventions (other rooms with at least "healthier" foam furniture but more potential building contamination; n = 28). In multilevel regression models, rooms with full "healthier" materials interventions had 78% lower dust levels of PFAS. Rooms with full "healthier" interventions also had 65% lower OPE levels in dust than rooms with no intervention (p < 0.01) and 45% lower PBDEs than rooms with only partial interventions (p< 0.10), adjusted for covariates related to insulation, electronics, and furniture. Bromine loadings from electronics in rooms were assocd. with PBDE concns. in dust (p < 0.05), and the presence of exposed insulation was assocd. with OPE dust concns. (p < 0.001). Full "healthier" materials renovations successfully reduced chem. classes in dust. Future interventions should address electronics, insulation, and building cross-contamination.
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    Miyake, Y.; Yamashita, N.; So, M. K.; Rostkowski, P.; Taniyasu, S.; Lam, P. K. S.; Kannan, K. Trace Analysis of Total Fluorine in Human Blood Using Combustion Ion Chromatography for Fluorine: A Mass Balance Approach for the Determination of Known and Unknown Organofluorine Compounds. J. Chromatogr. A 2007, 1154 (1–2), 214– 221,  DOI: 10.1016/j.chroma.2007.03.084
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    Trace analysis of total fluorine in human blood using combustion ion chromatography for fluorine: A mass balance approach for the determination of known and unknown organofluorine compounds
    Miyake, Yuichi; Yamashita, Nobuyoshi; So, Man Ka; Rostkowski, Pawel; Taniyasu, Sachi; Lam, Paul K. S.; Kannan, Kurunthachalam
    Journal of Chromatography A (2007), 1154 (1-2), 214-221CODEN: JCRAEY; ISSN:0021-9673. (Elsevier B.V.)
    The no. of perfluorochems. (PFCs) that have been found in biol. and environmental matrixes is increasing as anal. stds. and methods evolve. Perfluorooctanesulfonate (PFOS) and perfluorooctanoate (PFOA) constitute only a fraction of the total suite of PFCs found in environmental and biol. matrixes. A robust method and approach is needed to evaluate the mass of fluorinated compds. in biol. matrixes. In this study, we developed a method to measure total fluorine (TF) and org. fluorine (TOF) in human blood matrixes using combustion ion chromatog. (CIC). Blood matrixes (whole blood, serum, and plasma) were analyzed in bulk to det. TF. An aliquot of the blood was also extd. with org. solvents such as methyl-tert-Bu ether (MTBE) and hexane, and org. and aq. exts. were sepd., to fractionate organofluorines from inorg. fluorine. The org. layer was analyzed for TF by CIC, and for known PFCs by high performance liq. chromatog.-tandem mass spectrometry (HPLC-MS/MS). PFCs measured by HPLC-MS/MS accounted for >80% of the TF in the org. fraction. The aq. fraction contained inorg. fluorine and other non-extractable organofluorines. However, in the bulk sample, fluoride and non-extractable organofluorines accounted for >70% of the TF in blood samples from the general population. In occupationally exposed individuals, known organofluorines accounted for a major proportion of the TF. These results suggest the existence of yet uncharacterized fluorine fraction in human blood. Further studies are needed to characterize the aq. fraction that contains inorg. fluorine and non-extractable forms of fluorine.
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    Ritter, E. E.; Dickinson, M. E.; Harron, J. P.; Lunderberg, D. M.; DeYoung, P. A.; Robel, A. E.; Field, J. A.; Peaslee, G. F. PIGE as a Screening Tool for Per- and Polyfluorinated Substances in Papers and Textiles. Nucl. Instruments Methods Phys. Res. Sect. B Beam Interact. with Mater. Atoms 2017, 407, 47– 54,  DOI: 10.1016/j.nimb.2017.05.052
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    PIGE as a screening tool for Per- and polyfluorinated substances in papers and textiles
    Ritter, Evelyn E.; Dickinson, Margaret E.; Harron, John P.; Lunderberg, David M.; DeYoung, Paul A.; Robel, Alix E.; Field, Jennifer A.; Peaslee, Graham F.
    Nuclear Instruments & Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms (2017), 407 (), 47-54CODEN: NIMBEU; ISSN:0168-583X. (Elsevier B.V.)
    Per- and polyfluoroalkyl substances (PFASs) comprise a large array of man-made fluorinated chems. It is an emerging chem. class of concern because many PFASs are environmentally persistent and some have known ecol. and human toxicity. Consumer products treated with PFASs result in human exposure to PFASs through inhalation, ingestion, and environmental exposure to emissions from wastewater or from landfills. A rapid screening method based on total fluorine was developed and applied to quantify PFASs on consumer papers and textiles. Particle-Induced Gamma Ray Emission (PIGE) spectroscopy provides a non-destructive and quant. measurement of total fluorine on papers and textiles. This technique is both rapid and sensitive, with a limit of detection (LOD) of 13 nmol F/cm2 for papers and 24-45 nmol F/cm2 for textiles, with reproducibility of ±12% RSD for both. PIGE is a high throughput (>20 samples/h typically) method that was applied to 50 papers and 50 textiles in commerce to demonstrate the method.
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    Schultes, L.; Peaslee, G. F.; Brockman, J. D.; Majumdar, A.; McGuinness, S. R.; Wilkinson, J. T.; Sandblom, O.; Ngwenyama, R. A.; Benskin, J. P. Total Fluorine Measurements in Food Packaging: How Do Current Methods Perform?. Environ. Sci. Technol. Lett. 2019, 6 (2), 73– 78,  DOI: 10.1021/acs.estlett.8b00700
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    22
    Total fluorine measurements in food packaging: How do current methods perform?
    Schultes, Lara; Peaslee, Graham F.; Brockman, John D.; Majumdar, Ashabari; McGuinness, Sean R.; Wilkinson, John T.; Sandblom, Oskar; Ngwenyama, Ruth A.; Benskin, Jonathan P.
    Environmental Science & Technology Letters (2019), 6 (2), 73-78CODEN: ESTLCU; ISSN:2328-8930. (American Chemical Society)
    Per- and polyfluoroalkyl substances (PFASs) represent a class of more than 4000 compds. Their large no. and structural diversity pose a considerable challenge to anal. chemists. Measurement of total fluorine in environmental samples and consumer products is therefore crit. for rapidly screening for PFASs and for assessing the fraction of unexplained fluorine(i.e., fluorine mass balance). Here we compare three emerging anal. techniques for total fluorine detn.: combustion ion chromatog. (CIC), particle-induced γ-ray emission spectroscopy (PIGE), and instrumental neutron activation anal. (INAA). Application of each method to a certified ref. material (CRM), spiked filters, and representative food packaging samples revealed good accuracy and precision. INAA and PIGE had the advantage of being nondestructive, while CIC displayed the lowest detection limits. Inconsistencies between the methods arose due to the high aluminum content in the CRM, which precluded its anal. by INAA, and sample heterogeneity (i.e., coating on the surface of the material), which resulted in higher values from the surface measurement technique PIGE compared to the values from the bulk vol. techniques INAA and CIC. Comparing CIC-based extractable org. fluorine to target PFAS measurements of food packaging samples by liq. chromatog.-tandem mass spectrometry revealed large amts. of unidentified org. fluorine not captured by compd.-specific anal.
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    De Silva, A. O.; Armitage, J. M.; Bruton, T. A.; Dassuncao, C.; Heiger-Bernays, W.; Hu, X. C.; Kärrman, A.; Kelly, B.; Ng, C.; Robuck, A.; Sun, M.; Webster, T. F.; Sunderland, E. M. PFAS Exposure Pathways for Humans and Wildlife: A Synthesis of Current Knowledge and Key Gaps in Understanding. Environ. Toxicol. Chem. 2021, 40 (3), 631– 657,  DOI: 10.1002/etc.4935
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    PFAS Exposure Pathways for Humans and Wildlife: A Synthesis of Current Knowledge and Key Gaps in Understanding
    De Silva, Amila O.; Armitage, James M.; Bruton, Thomas A.; Dassuncao, Clifton; Heiger-Bernays, Wendy; Hu, Xindi C.; Kaerrman, Anna; Kelly, Barry; Ng, Carla; Robuck, Anna; Sun, Mei; Webster, Thomas F.; Sunderland, Elsie M.
    Environmental Toxicology and Chemistry (2021), 40 (3), 631-657CODEN: ETOCDK; ISSN:0730-7268. (Wiley-Blackwell)
    A review. We synthesize current understanding of the magnitudes and methods for assessing human and wildlife exposures to poly- and perfluoroalkyl substances (PFAS). Most human exposure assessments have focused on 2 to 5 legacy PFAS, and wildlife assessments are typically limited to targeted PFAS (up to ∼30 substances). However, shifts in chem. prodn. are occurring rapidly, and targeted methods for detecting PFAS have not kept pace with these changes. Total fluorine measurements complemented by suspect screening using high-resoln. mass spectrometry are thus emerging as essential tools for PFAS exposure assessment. Such methods enable researchers to better understand contributions from precursor compds. that degrade into terminal perfluoroalkyl acids. Available data suggest that diet is the major human exposure pathway for some PFAS, but there is large variability across populations and PFAS compds. Addnl. data on total fluorine in exposure media and the fraction of unidentified organofluorine are needed. Drinking water has been established as the major exposure source in contaminated communities. As water supplies are remediated, for the general population, exposures from dust, personal care products, indoor environments, and other sources may be more important. A major challenge for exposure assessments is the lack of statistically representative population surveys. For wildlife, bioaccumulation processes differ substantially between PFAS and neutral lipophilic org. compds., prompting a reevaluation of traditional bioaccumulation metrics. There is evidence that both phospholipids and proteins are important for the tissue partitioning and accumulation of PFAS. New mechanistic models for PFAS bioaccumulation are being developed that will assist in wildlife risk evaluations.
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    Robel, A. E.; Marshall, K.; Dickinson, M.; Lunderberg, D.; Butt, C.; Peaslee, G.; Stapleton, H. M.; Field, J. A. Closing the Mass Balance on Fluorine on Papers and Textiles. Environ. Sci. Technol. 2017, 51 (16), 9022– 9032,  DOI: 10.1021/acs.est.7b02080
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    24
    Closing the Mass Balance on Fluorine on Papers and Textiles
    Robel, Alix E.; Marshall, Kristin; Dickinson, Margaret; Lunderberg, David; Butt, Craig; Peaslee, Graham; Stapleton, Heather M.; Field, Jennifer A.
    Environmental Science & Technology (2017), 51 (16), 9022-9032CODEN: ESTHAG; ISSN:0013-936X. (American Chemical Society)
    Paper and textiles treated with per- and polyfluoroalkyl substances (PFAS) are sources of human and environmental exposure. Data for individual PFAS, e.g., perfluorooctanesulfonate (PFOS) and perfluorooctanoate (PFOA), are not placed in the context of total F for paper and textiles. Gas chromatog./mass spectrometry (GC/MS) and liq. chromatog./tandem mass spectrometry (LC/MS-MS) quantified volatile and ionic PFAS, resp.; the total oxidizable precursor (TOP) assay quantified precursors which form perfluoroalkyl carboxylates. Molar sums of PFAS obtained by GC/MS, LC/MS-/MS, and precursors were compared to total F (nmol F/cm2) detd. by particle-induced gamma ray emission (PIGE) spectroscopy, measured before and after extn. Volatile and ionic PFAS and unknown precursors accounted for 0-2.2%, 0-0.41%, and 0.021-14%, resp., of total nmol F/cm2 detd. by PIGE. Following extn., paper and textiles retained 64 ± 28% to 110 ± 30% of the original nmol F/cm2 as detd. by PIGE, indicating the majority of F remains assocd. with the paper and textiles. The sum of PFAS in volatile, ionic, and precursor fractions, and total F post-extn. indicated that mass balance was achieved (within anal. error) of the initial total F measured by PIGE.
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  25. 25
    Schultes, L.; Vestergren, R.; Volkova, K.; Westberg, E.; Jacobson, T.; Benskin, J. P. Per- and Polyfluoroalkyl Substances and Fluorine Mass Balance in Cosmetic Products from the Swedish Market: Implications for Environmental Emissions and Human Exposure. Environ. Sci. Process. Impacts 2018, 20 (12), 1680– 1690,  DOI: 10.1039/C8EM00368H
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    25
    Per- and polyfluoroalkyl substances and fluorine mass balance in cosmetic products from the Swedish market: implications for environmental emissions and human exposure
    Schultes, Lara; Vestergren, Robin; Volkova, Kristina; Westberg, Emelie; Jacobson, Therese; Benskin, Jonathan P.
    Environmental Science: Processes & Impacts (2018), 20 (12), 1680-1690CODEN: ESPICZ; ISSN:2050-7895. (Royal Society of Chemistry)
    Per-and polyfluoroalkyl substances (PFASs) are a diverse class of < 4700 chems. used in com. products and industrial processes. Concerns surrounding PFASs are principally due to their widespread occurrence in humans and the environment and links to adverse health effects. One of the lesser known uses for PFASs is in cosmetic products (CPs) which come into contact with the skin (e.g. hair products, powders, sunblocks, etc.). In the present work, thirty-one CPs from five product categories (cream, foundation, pencil, powder and shaving foam) were analyzed for 39 PFASs by liq. chromatog.-tandem mass spectrometry, as well as extractable org. fluorine (EOF) and total fluorine (TF) by combustion ion chromatog. (CIC). This multi-platform approach enabled detn. of the fraction of fluorine accounted for by known PFASs (i.e. fluorine mass balance). Foundations and powders contained 25 different PFASs with the most frequently detected being perfluorinated carboxylic acids (perfluoroheptanoic acid and perfluorohexanoic acid) and polyfluoroalkyl phosphate esters (PAPs). U+03C314PAP concns. up to 470μg g-1 were measured in products listing mixts. of PAPs as an ingredient. For all samples, U+03C3 39PFAS concns. only explained a small fraction of the EOF and TF, pointing to the presence of unknown org. and/or inorg. fluorinated substances, including polymers. While creams, pencil and shaving foams did not contain measurable concns. of any of the 39 PFASs targeted here, CIC revealed high to moderate TF content. Overall, these data highlight the need for further investigations into the occurrence of PFASs in CPs and their importance with regards to human and environmental exposure.
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  26. 26
    Peaslee, G. F.; Wilkinson, J. T.; McGuinness, S. R.; Tighe, M.; Caterisano, N.; Lee, S.; Gonzales, A.; Roddy, M.; Mills, S.; Mitchell, K. Another Pathway for Firefighter Exposure to Per- and Polyfluoroalkyl Substances: Firefighter Textiles. Environ. Sci. Technol. Lett. 2020, 7 (8), 594– 599,  DOI: 10.1021/acs.estlett.0c00410
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    Another Pathway for Firefighter Exposure to Per- and Polyfluoroalkyl Substances: Firefighter Textiles
    Peaslee, Graham F.; Wilkinson, John T.; McGuinness, Sean R.; Tighe, Meghanne; Caterisano, Nicholas; Lee, Seryeong; Gonzales, Alec; Roddy, Matthew; Mills, Simon; Mitchell, Krystle
    Environmental Science & Technology Letters (2020), 7 (8), 594-599CODEN: ESTLCU; ISSN:2328-8930. (American Chemical Society)
    Occupational exposure to aq. film-forming foams (AFFF) can lead to elevated concns. of per- and polyfluorinated alkyl substances (PFAS) in firefighter blood sera. AFFF are also one PFAS exposure source in the general population due to their environmental persistence and soly. in groundwater. Due to documented PFAS adverse health effects, the primary concern to date for the fire services centered on repeated AFFF use and exposure. This work presents an addnl. PFAS exposure source for firefighters: PFAS shed from their protective clothing. Textiles in firefighter turn-out gear had high total F concns. (up to 2%); individual PFAS were identified and measured on new and used firefighting turn-out gear. Used gear showed lower PFAS concn. and increased migration to untreated material. Textile storage area dust measurements also suggested direct loss of PFAS from the textile fluoropolymers. Since PFAS shed from turn-out gear textiles are more mobile, they represent another exposure source for firefighters which warrants addnl. study.
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  27. 27
    Tokranov, A. K.; Nishizawa, N.; Amadei, C. A.; Zenobio, J. E.; Pickard, H. M.; Allen, J. G.; Vecitis, C. D.; Sunderland, E. M. How Do We Measure Poly- and Perfluoroalkyl Substances (PFASs) at the Surface of Consumer Products?. Environ. Sci. Technol. Lett. 2018, 6, 38,  DOI: 10.1021/acs.estlett.8b00600
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    Poothong, S.; Papadopoulou, E.; Padilla-Sánchez, J. A.; Thomsen, C.; Haug, L. S. Multiple Pathways of Human Exposure to Poly- and Perfluoroalkyl Substances (PFASs): From External Exposure to Human Blood. Environ. Int. 2020, 134, 105244,  DOI: 10.1016/j.envint.2019.105244
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    Multiple pathways of human exposure to poly- and perfluoroalkyl substances (PFASs): From external exposure to human blood
    Poothong, Somrutai; Papadopoulou, Eleni; Padilla-Sanchez, Juan Antonio; Thomsen, Cathrine; Haug, Line Smaastuen
    Environment International (2020), 134 (), 105244CODEN: ENVIDV; ISSN:0160-4120. (Elsevier Ltd.)
    This study aimed to characterize the exposure to PFASs from diet, house dust, indoor air, and dermal contact and the relative contribution from different external exposure pathways to human serum concns. Concns. of PFAAs and PFAA precursors in house dust, indoor air, hand wipes, foods and drinks were utilized to est. the daily intakes. Dietary exposure from ingestion of food and drinks was in general the predominant exposure pathway, followed by exposure from ingestion of house dust, inhalation of indoor air, and dermal absorption, but considerable variations were obsd. among individuals. House dust ingestion and indoor air inhalation contributed most to the total intakes for some participants, for which most of them were among the 20% participants with the highest total estd. intakes. Some statistical significant assocns. between concns. of PFASs measured in serum and estd. intakes were obsd. Measured serum concns. and modelled serum concns. based on external exposure ests. were in the same order of magnitude for PFOS, PFHxS, PFOA, and PFNA, but only PFOA concns. were comparable, 1.9 and 2.0 ng mL-1 for obsd. and modelled serum concns., resp. The estd. daily intakes of PFASs in this study were lower than the health-based guidance values, e.g. the tolerable weekly intakes derived by EFSA. This study underlines the importance of performing studies considering multiple exposure pathways on an individual basis.
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  29. 29
    Mitro, S. D.; Dodson, R. E.; Singla, V.; Adamkiewicz, G.; Elmi, A. F.; Tilly, M. K.; Zota, A. R. Consumer Product Chemicals in Indoor Dust: A Quantitative Meta-Analysis of U.S. Studies. Environ. Sci. Technol. 2016, 50 (19), 10661– 10672,  DOI: 10.1021/acs.est.6b02023
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    29
    Consumer Product Chemicals in Indoor Dust: A Quantitative Meta-analysis of U.S. Studies
    Mitro, Susanna D.; Dodson, Robin E.; Singla, Veena; Adamkiewicz, Gary; Elmi, Angelo F.; Tilly, Monica K.; Zota, Ami R.
    Environmental Science & Technology (2016), 50 (19), 10661-10672CODEN: ESTHAG; ISSN:0013-936X. (American Chemical Society)
    Indoor dust is a reservoir for com. consumer product chems., including many compds. with known or suspected health effects; however, most dust exposure studies measure few chems. in small samples. This work systematically searched the US indoor dust literature on phthalates, replacement flame retardants (RFR), perfluoroalkyl substances (PFAS), synthetic fragrances, and environmental phenols, and estd. pooled geometric means (GM) and 95% confidence intervals for 45 chems. measured in ≥3 datasets. Pooled GM calcd. residential intake from dust ingestion, inhalation, and dermal uptake from air, then hazard traits from the Safer Consumer Products Candidate Chem. List were identified to rank and contextualize these results. Results indicated US indoor dust consistently contains chems. from multiple classes. Phthalates occurred in the highest concns., followed by phenols, RFR, fragrance, and PFAS; several phthalates and RFR had the highest residential intakes. Many chems. in dust share hazard traits, e.g., reproductive and endocrine toxicity. Recommendations are made to maximize study comparability and advance indoor exposure science. This information is crit. in shaping future exposure and health studies, particularly related to cumulative exposure, and providing evidence for intervention development and public policy.
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  30. 30
    Ruyle, B. J.; Pickard, H. M.; LeBlanc, D. R.; Tokranov, A. K.; Thackray, C. P.; Hu, X. C.; Vecitis, C. D.; Sunderland, E. M. Isolating the AFFF Signature in Coastal Watersheds Using Oxidizable PFAS Precursors and Unexplained Organofluorine. Environ. Sci. Technol. 2021, 55 (6), 3686– 3695,  DOI: 10.1021/acs.est.0c07296
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    Isolating the AFFF signature in coastal watersheds using oxidizable PFAS precursors and unexplained organofluorine
    Ruyle, Bridger J.; Pickard, Heidi M.; LeBlanc, Denis R.; Tokranov, Andrea K.; Thackray, Colin P.; Hu, Xindi C.; Vecitis, Chad D.; Sunderland, Elsie M.
    Environmental Science & Technology (2021), 55 (6), 3686-3695CODEN: ESTHAG; ISSN:0013-936X. (American Chemical Society)
    Water supplies for millions of U.S. individuals exceed max. contaminant levels for per- and polyfluoroalkyl substances (PFAS). Contemporary and legacy use of aq. film forming foams (AFFF) is a major contamination source. However, diverse PFAS sources are present within watersheds, making it difficult to isolate their predominant origins. Here we examine PFAS source signatures among six adjacent coastal watersheds on Cape Cod, MA, U.S.A. using multivariate clustering techniques. A distinct signature of AFFF contamination enriched in precursors with six perfluorinated carbons (C6) was identified in watersheds with an AFFF source, while others were enriched in C4 precursors. Principal component anal. of PFAS compn. in impacted watersheds showed a decline in precursor compn. relative to AFFF stocks and a corresponding increase in terminal perfluoroalkyl sulfonates with < C6 but not those with ≥ C6. Prior work shows that in AFFF stocks, all extractable organofluorine (EOF) can be explained by targeted PFAS and precursors inferred using Bayesian inference on the total oxidizable precursor assay. Using the same techniques for the first time in impacted watersheds, we find that only 24%-63% of the EOF can be explained by targeted PFAS and oxidizable precursors. Our work thus indicates the presence of large non-AFFF organofluorine sources in these coastal watersheds.
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  31. 31
    Young, A. S.; Sparer-Fine, E. H.; Pickard, H. M.; Sunderland, E. M.; Peaslee, G. F.; Allen, J. G. Per- and Polyfluoroalkyl Substances (PFAS) and Total Fluorine in Fire Station Dust. J. Expo. Sci. Environ. Epidemiol 2021, 930,  DOI: 10.1038/s41370-021-00288-7
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    31
    Per- and polyfluoroalkyl substances (PFAS) and total fluorine in fire station dust
    Young, Anna S.; Sparer-Fine, Emily H.; Pickard, Heidi M.; Sunderland, Elsie M.; Peaslee, Graham F.; Allen, Joseph G.
    Journal of Exposure Science & Environmental Epidemiology (2021), 31 (5), 930-942CODEN: JESEBS; ISSN:1559-0631. (Nature Portfolio)
    Abstr.: Per- and polyfluoroalkyl substances (PFAS) are a class of over 4700 fluorinated compds. used in industry and consumer products. Studies have highlighted the use of aq. film-forming foams (AFFFs) as an exposure source for firefighters, but little is known about PFAS occurrence inside fire stations, where firefighters spend most of their shifts. In this study, we aimed to characterize PFAS concns. and sources inside fire stations. We measured 24 PFAS (using LC-MS/MS) and total fluorine (using particle-induced gamma ray emission) in dust from multiple rooms of 15 Massachusetts stations, many of which (60%) no longer use PFAS-contg. AFFF at all and the rest of which only use it very rarely. Compared to station living rooms, turnout gear locker rooms had higher dust levels of total fluorine (p < 0.0001) and three PFAS: perfluorohexanoate (PFHxA), perfluoroheptanoate (PFHpA), and perfluorodecanoate (PFDoDA) (p < 0.05). These PFAS were also found on six wipes of station turnout gear. By contrast, the dominant PFAS in living rooms was N-Et perfluorooctane sulfonamidoacetic acid (N-MeFOSAA), a precursor to perfluorooctane sulfonate (PFOS) that still persists despite phase-outs almost two decades ago. The Σ24 PFAS accounted for less than 2% of fluorine in dust (n = 39), suggesting the potential presence of unknown PFAS. Turnout gear may be an important PFAS source in stations due to intentional additives and/or contamination from firefighting activities.
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  32. 32
    Aro, R.; Carlsson, P.; Vogelsang, C.; Kärrman, A.; Yeung, L. W. Y. Fluorine Mass Balance Analysis of Selected Environmental Samples from Norway. Chemosphere 2021, 283, 131200,  DOI: 10.1016/j.chemosphere.2021.131200
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    Fluorine mass balance analysis of selected environmental samples from Norway
    Aro, Rudolf; Carlsson, Pernilla; Vogelsang, Christian; Kaerrman, Anna; Yeung, Leo WY.
    Chemosphere (2021), 283 (), 131200CODEN: CMSHAF; ISSN:0045-6535. (Elsevier Ltd.)
    The presence of unidentified organofluorine compds. (UOF) has been investigated in recent publication, but their environmental occurrence is still poorly understood. Fluorine mass balance anal. was performed on environmental samples from lake Mjosa and river Alna (surface water (n = 9), sediment (n = 5) and fish liver (n = 4)) and sewage samples from Oslo (n = 5), to reveal to the fraction of UOF. In samples that had extractable organofluorine (EOF) concns. above the limit of detection (LoD), more than 70% of their EOF could not be accounted for by the 37 PFAS monitored in this study. The surface water samples from lake Mjosa had EOF concns. several times higher than what has been reported elsewhere in Nordic nations. The flux of EOF in river Alna and selected sewage pipes revealed that it was 1-2 orders of magnitude higher than the flux of the measured PFAS. The elevated concns. of EOF in all samples pose a potential health and environmental hazard, as their compn. remains mostly unknown.
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  33. 33
    Yeung, L. W. Y.; Miyake, Y.; Li, P.; Taniyasu, S.; Kannan, K.; Guruge, K. S.; Lam, P. K. S.; Yamashita, N. Comparison of Total Fluorine, Extractable Organic Fluorine and Perfluorinated Compounds in the Blood of Wild and Pefluorooctanoate (PFOA)-Exposed Rats: Evidence for the Presence of Other Organofluorine Compounds. Anal. Chim. Acta 2009, 635 (1), 108– 114,  DOI: 10.1016/j.aca.2009.01.004
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    Comparison of total fluorine, extractable organic fluorine and perfluorinated compounds in the blood of wild and pefluorooctanoate (PFOA)-exposed rats: Evidence for the presence of other organofluorine compounds
    Yeung, Leo W. Y.; Miyake, Yuichi; Li, Peng; Taniyasu, Sachi; Kannan, Kurunthachalam; Guruge, Keerthi S.; Lam, Paul K. S.; Yamashita, Nobuyoshi
    Analytica Chimica Acta (2009), 635 (1), 108-114CODEN: ACACAM; ISSN:0003-2670. (Elsevier B.V.)
    The widespread occurrence and environmental persistence of perfluorinated compds. (PFCs) received worldwide attention recently. Exhaustive anal. of all fluorinated compds. in an environmental sample can be daunting because of the constraints in the availability of anal. stds. and extn. methods. Combustion ion chromatog. technique for trace fluorine anal. was used to assess the concns. of known PFCs (e.g., PFOS, PFOA) and total fluorine (TF) in the blood of wild rats collected from Japan. The technique was further validated using tissues from PFOA-exposed rats. Six PFCs (PFOS, PFOSA, PFUnDA, PFDA, PFNA, and PFOA) were detected in all of the wild rat blood samples. Concns. of extractable org. fluorine (EOF) in fraction 1 (Fr1; MTBE extn.) of wild rats ranged 60.9-134 ng F mL-1, while those in fraction 2 (Fr2; hexane) were below LOQ (32 ng F mL-1); TF concns. in the blood of wild rats ranged from 59.9-192 ng F mL-1. The contribution of known PFCs in EOF-Fr1 (MTBE) varied from 9% to 89% (56% on av.), and known PFC concns. in TF content were less than 25%. In contrast, TF concns. in the blood of PFOA-exposed rats ranged from 46900 to 111000 ng F mL-1, with PFOA contributing over 90% of TF. A comparison of results from the samples analyzed in this study and the literature revealed three distinct groups with PFOA/known PFC and TF levels (i.e., wild rats and general population, occupationally exposed workers, and PFOA-exposed lab. rats). The mass balance anal. of the different forms of fluorine in blood suggested the presence of other forms of org. fluorine in addn. to known PFCs.
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    Miyake, Y.; Yamashita, N.; Rostkowski, P.; So, M. K.; Taniyasu, S.; Lam, P. K. S.; Kannan, K. Determination of Trace Levels of Total Fluorine in Water Using Combustion Ion Chromatography for Fluorine: A Mass Balance Approach to Determine Individual Perfluorinated Chemicals in Water. J. Chromatogr. A 2007, 1143 (1–2), 98– 104,  DOI: 10.1016/j.chroma.2006.12.071
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    Determination of trace levels of total fluorine in water using combustion ion chromatography for fluorine: A mass balance approach to determine individual perfluorinated chemicals in water
    Miyake, Yuichi; Yamashita, Nobuyoshi; Rostkowski, Pawel; So, Man Ka; Taniyasu, Sachi; Lam, Paul K. S.; Kannan, Kurunthachalam
    Journal of Chromatography A (2007), 1143 (1-2), 98-104CODEN: JCRAEY; ISSN:0021-9673. (Elsevier B.V.)
    Perfluorinated compds. (PFC), e.g., perfluorooctanesulfonate (PFOS) and perfluorooctanoate (PFOA), have received worldwide attention due to their environmental persistence and widespread distribution. Due to a lack of robust anal. methods and stds. to detect all the PFC and their precursors and metabolic intermediates, a mass balance approach involving detn. of total F (TF), followed by sample fractionation sep. det. inorg. and org. F, is needed. This work developed a method to det. low μg/L concns. TF in seawater. Seawater samples were fractionated into org. and inorg. fractions by extn. with org. solvents, which were then analyzed for TF, extractable org. F (EOF) and inorg. F (IF, i.e., F-). Concns. of known perfluorinated compds. (PFC) including PFOS and PFOA were also detd. in water by liq. chromatog.-tandem mass spectrometry (LC-MS/MS) to calc. the fraction of F contributed by PFC to TF. A major proportion of F in seawater was in the form of F- (>90% at sites not affected by direct discharges). Nevertheless, within the organofluorine fraction, a major percentage (60-90%) of F still remains unknown in water samples, suggesting the occurrence of other fluorinated acids in addn. to known perfluorinated acids. Further studies are needed to identify and quantify unidentified organofluorines in seawater. Mass balance anal. of total org. F (TOF) and EOF is important, to understand fluorinated compd. environmental transport and fate and to identify sources of unidentified fluorinated compds.
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    Weber, A. K.; Barber, L. B.; LeBlanc, D. R.; Sunderland, E. M.; Vecitis, C. D. Geochemical and Hydrologic Factors Controlling Subsurface Transport of Poly- and Perfluoroalkyl Substances, Cape Cod, Massachusetts. Environ. Sci. Technol. 2017, 51 (8), 4269– 4279,  DOI: 10.1021/acs.est.6b05573
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    Geochemical and Hydrologic Factors Controlling Subsurface Transport of Poly- and Perfluoroalkyl Substances, Cape Cod, Massachusetts
    Weber, Andrea K.; Barber, Larry B.; LeBlanc, Denis R.; Sunderland, Elsie M.; Vecitis, Chad D.
    Environmental Science & Technology (2017), 51 (8), 4269-4279CODEN: ESTHAG; ISSN:0013-936X. (American Chemical Society)
    Growing evidence that certain poly- and perfluoroalkyl substances (PFASs) are assocd. with neg. human health effects prompted the U.S. Environmental Protection Agency to issue lifetime drinking water health advisories for perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS) in 2016. Given that groundwater is a major source of drinking water, the main objective of this work was to investigate geochem. and hydrol. processes governing the subsurface transport of PFASs at a former fire training area (FTA) on Cape Cod, Massachusetts, where PFAS-contg. aq. film-forming foams were used historically. A total of 148 groundwater samples and 4 sediment cores were collected along a 1200-m-long downgradient transect originating near the FTA, and analyzed for PFAS content. The results indicate that unsatd. zones at the FTA and at hydraulically downgradient former domestic wastewater effluent infiltration beds both act as continuous PFAS sources to the groundwater despite 18 and 20 years of inactivity, resp. Historically different PFAS sources are evident from contrasting PFAS compn. near the water table below the FTA and wastewater-infiltration beds. Results from total oxidizable precursor assays conducted using groundwater samples collected throughout the plume suggest that some perfluoroalkyl acid precursors at this site are transporting with perfluoroalkyl acids.
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    Shoari, N.; Dubé, J.-S. Toward Improved Analysis of Concentration Data: Embracing Nondetects. Environ. Toxicol. Chem. 2018, 37 (3), 643– 656,  DOI: 10.1002/etc.4046
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    Toward improved analysis of concentration data: Embracing nondetects
    Shoari, Niloofar; Dube, Jean-Sebastien
    Environmental Toxicology and Chemistry (2018), 37 (3), 643-656CODEN: ETOCDK; ISSN:0730-7268. (Wiley-Blackwell)
    Various statistical tests on concn. data serve to support decision-making regarding characterization and monitoring of contaminated media, assessing exposure to a chem., and quantifying the assocd. risks. However, the routine statistical protocols cannot be directly applied because of challenges arising from nondetects or left-censored observations, which are concn. measurements below the detection limit of measuring instruments. Despite the existence of techniques based on survival anal. that can adjust for nondetects, these are seldom taken into account properly. A comprehensive review of the literature showed that managing policies regarding anal. of censored data do not always agree and that guidance from regulatory agencies may be outdated. Therefore, researchers and practitioners commonly resort to the most convenient way of tackling the censored data problem by substituting nondetects with arbitrary consts. prior to data anal., although this is generally regarded as a bias-prone approach. Hoping to improve the interpretation of concn. data, the present article aims to familiarize researchers in different disciplines with the significance of left-censored observations and provides theor. and computational recommendations (under both frequentist and Bayesian frameworks) for adequate anal. of censored data. In particular, the present article synthesizes key findings from previous research with respect to 3 noteworthy aspects of inferential statistics: estn. of descriptive statistics, hypothesis testing, and regression anal. Environ Toxicol Chem 2018;9999:1-14. © 2017 SETAC.
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    Johnson, N.; Shelton, B. J.; Hopenhayn, C.; Tucker, T. T.; Unrine, J. M.; Huang, B.; Christian, W.; Zhang, Z.; Shi, X.; Li, L. Concentrations of Arsenic, Chromium, and Nickel in Toenail Samples from Appalachian Kentucky Residents. J. Environ. Pathol. Toxicol. Oncol. Off. organ Int. Soc. Environ. Toxicol. Cancer 2011, 30 (3), 213– 223,  DOI: 10.1615/JEnvironPatholToxicolOncol.v30.i3.40
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    Concentrations of arsenic, chromium, and nickel in toenail samples from Appalachian Kentucky residents
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Cite this: Environ. Sci. Technol. 2022, 56, 23, 17090–17099
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  • Abstract

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    Figure 1

    Figure 1. Concentrations of the sum of 15 targeted PFAS (ng/g) (left panel) and extractable organic fluorine (EOF) (ng F/g) (right panel) in 24 dust samples from rooms with conventional or “healthier” building materials.

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    Figure 2

    Figure 2. Median concentrations (ng F/g) of total fluorine, extractable organic fluorine (EOF), and calculated organic fluorine equivalents based on measured PFAS in dust samples from n = 24 rooms with conventional or “healthier” materials.

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      Continuous non-marine inputs of per- and polyfluoroalkyl substances to the High Arctic: a multi-decadal temporal record
      Pickard, Heidi M.; Criscitiello, Alison S.; Spencer, Christine; Sharp, Martin J.; Muir, Derek C. G.; De Silva, Amila O.; Young, Cora J.
      Atmospheric Chemistry and Physics (2018), 18 (7), 5045-5058CODEN: ACPTCE; ISSN:1680-7324. (Copernicus Publications)
      Perfluoroalkyl acids (PFAAs) are persistent, in some cases, bioaccumulative compds. found ubiquitously within the environment. They can be formed from the atm. oxidn. of volatile precursor compds. and undergo long-range transport (LRT) through the atm. and ocean to remote locations. Ice caps preserve a temporal record of PFAA deposition making them useful in studying the atm. trends in LRT of PFAAs in polar or mountainous regions, as well as in understanding major pollutant sources and prodn. changes over time. A 15m ice core representing 38 years of deposition (1977-2015) was collected from the Devon Ice Cap in Nunavut, providing us with the first multi-decadal temporal ice record in PFAA deposition to the Arctic. Ice core samples were concd. using solid phase extn. and analyzed by liq. and ion chromatog. methods. Both perfluoroalkyl carboxylic acids (PFCAs) and perfluoroalkyl sulfonic acids (PFSAs) were detected in the samples, with fluxes ranging from <LOD to 141 ng m-2 yr-1. Our results demonstrate that the PFCAs and perfluorooctane sulfonate (PFOS) have continuous and increasing deposition on the Devon Ice Cap, despite recent North American and international regulations and phaseouts. We propose that this is the result of on-going manuf., use and emissions of these compds., their precursors and other newly unidentified compds. in regions outside of North America. By modeling air mass transport densities, and comparing temporal trends in deposition with prodn. changes of possible sources, we find that Eurasian sources, particularly from Continental Asia, are large contributors to the global pollutants impacting the Devon Ice Cap. Comparison of PFAAs to their precursors and correlations of PFCA pairs showed that deposition of PFAAs is dominated by atm. formation from volatile precursor sources. Major ion anal. confirmed that marine aerosol inputs are unimportant to the long-range transport mechanisms of these compds. Assessments of deposition, homolog profiles, ion tracers, air mass transport models, and prodn. and regulation trends allow us to characterize the PFAA depositional profile on the Devon Ice Cap and further understand the LRT mechanisms of these persistent pollutants.
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    9. 9
      Yamashita, N.; Taniyasu, S.; Petrick, G.; Wei, S.; Gamo, T.; Lam, P. K. S.; Kannan, K. Perfluorinated Acids as Novel Chemical Tracers of Global Circulation of Ocean Waters. Chemosphere 2008, 70 (7), 1247– 1255,  DOI: 10.1016/j.chemosphere.2007.07.079
      9
      Perfluorinated acids as novel chemical tracers of global circulation of ocean waters
      Yamashita, Nobuyoshi; Taniyasu, Sachi; Petrick, Gert; Wei, Si; Gamo, Toshitaka; Lam, Paul K. S.; Kannan, Kurunthachalam
      Chemosphere (2008), 70 (7), 1247-1255CODEN: CMSHAF; ISSN:0045-6535. (Elsevier Ltd.)
      Perfluorinated acids (PFAs) such as perfluorooctanesulfonate (PFOS) and perfluorooctanoate (PFOA) are global environmental contaminants. The physicochem. properties of PFAs are unique in that they have high water solubilities despite the low reactivity of C-F bond, which also imparts high stability in the environment. Because of the high water solubilities, the open-ocean water column is suggested to be the final sink for PFOS and PFOA. However, little is known on the distribution of PFAs in the oceans around the world. We describe the horizontal (spatial) and vertical distribution of PFAs in ocean waters worldwide. PFOS and PFOA concns. in the North Atlantic Ocean ranged from 8.6 to 36 pg/L and from 52 to 338 pg/L, resp., whereas the corresponding concns. in the Mid Atlantic Ocean were 13-73 and 67-439 pg/L. These were completely different from the surface waters of the South Pacific Ocean and the Indian Ocean (overall range of <5-11 pg/L for PFOS and PFOA). Vertical profiles of PFAs in the marine water column were assocd. with the global ocean circulation theory. Vertical profiles of PFAs in water columns from the Labrador Sea reflected the influx of the North Atlantic Current in surface waters, the Labrador Current in subsurface waters, and the Denmark Strait Overflow Water in deep layers below 2000 m. Striking differences in the vertical and spatial distribution of PFAs, depending on the oceans, suggest that these persistent acids can serve as useful chem. tracers to allow us to study oceanic transport by major water currents. The results provide evidence that PFA concns. and profiles in the oceans adhere to a pattern consistent with the global Broecker's Conveyor Belt theory of open ocean water circulation.
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    10. 10
      Giesy, J. P.; Kannan, K. Global Distribution of Perfluorooctane Sulfonate in Wildlife. Environ. Sci. Technol. 2001, 35 (7), 1339– 1342,  DOI: 10.1021/es001834k
      10
      Global distribution of perfluorooctane sulfonate in wildlife
      Giesy, John P.; Kannan, Kurunthachalam
      Environmental Science and Technology (2001), 35 (7), 1339-1342CODEN: ESTHAG; ISSN:0013-936X. (American Chemical Society)
      The global distribution of perfluorooctanesulfonate (PFOS), a fluorinated org. contaminant. PFOS measured in the tissues of wildlife, including, fish, birds, and marine mammals is reported. Some of the species studied include bald eagles, polar bears, albatrosses, and various species of seals. Samples were collected from urbanized areas in North America, esp. the Great Lakes region and coastal marine areas and rivers, and Europe. Samples were also collected from a no. of more remote, less urbanized locations such as the Arctic and the North Pacific Oceans. The results demonstrated that PFOS is widespread in the environment. Concns. of PFOS in animals from relatively more populated and industrialized regions, such as the North American Great Lakes, Baltic Sea, and Mediterranean Sea, were greater than those in animals from remote marine locations. Fish-eating, predatory animals such as mink and bald eagles contained concns. of PFOS that were greater than the concns. in their diets. This suggests that PFOS can bioaccumulate to higher trophic levels of the food chain. Currently available data indicate that the concns. of PFOS in wildlife are less than those required to cause adverse effects in lab. animals.
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    11. 11
      Calafat, A. M.; Wong, L. Y.; Kuklenyik, Z.; Reidy, J. A.; Needham, L. L. Polyfluoroalkyl Chemicals in the U.S. Population: Data from the National Health and Nutrition Examination Survey (NHANES) 2003–2004 and Comparisons with NHANES 1999–2000. Environ. Health Perspect 2007, 115 (11), 1596– 1602,  DOI: 10.1289/ehp.10598
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      Polyfluoroalkyl chemicals in the U.S. population: data from the National Health and Nutrition Examination Survey 2003-2004 and comparisons with NHANES 1999-2000
      Calafat, Antonia M.; Wong, Lee-Yang; Kuklenyik, Zsuzsanna; Reidy, John A.; Needham, Larry L.
      Environmental Health Perspectives (2007), 115 (11), 1596-1602CODEN: EVHPAZ; ISSN:0091-6765. (U. S. Department of Health and Human Services, Public Health Services)
      Polyfluoroalkyl chems. (PFCs) have been used since the 1950s in numerous com. applications. Exposure of the general U.S. population to PFCs is widespread. Since 2002, the manufg. practices for PFCs in the United States have changed considerably. We aimed to assess exposure to perfluorooctane sulfonic acid (PFOS), perfluorooctanoic acid (PFOA), perfluorohexane sulfonic acid (PFHxS), perfluorononanoic acid (PFNA), and eight other PFCs in a representative 2003-2004 sample of the general U.S. population ≥ 12 years of age and to det. whether serum concns. have changed since the 1999-2000 National Health and Nutrition Examn. Survey (NHANES). By using automated solid-phase extn. coupled to isotope diln.-high-performance liq. chromatog.-tandem mass spectrometry, we analyzed 2094 serum samples collected from NHANES 2003-2004 participants. We detected PFOS, PFOA, PFHxS, and PFNA in >98% of the samples. Concns. differed by race/ethnicity and sex. Geometric mean concns. were significantly lower (approx. 32% for PFOS, 25% for PFOA, 10% for PFHxS) and higher (100%, PFNA) than the concns. reported in NHANES 1999-2000 (p < 0.001). In the general U.S. population in 2003-2004, PFOS, PFOA, PFHxS, and PFNA serum concns. were measurable in each demog. population group studied. Geometric mean concns. of PFOS, PFOA, and PFHxS in 2003-2004 were lower than in 1999-2000. The apparent redns. in concns. of PFOS, PFOA, and PFHxS most likely are related to discontinuation in 2002 of industrial prodn. by electrochem. fluorination of PFOS and related perfluorooctanesulfonyl fluoride compds.
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    12. 12
      Fenton, S. E.; Ducatman, A.; Boobis, A.; DeWitt, J. C.; Lau, C.; Ng, C.; Smith, J. S.; Roberts, S. M. Per- and Polyfluoroalkyl Substance Toxicity and Human Health Review: Current State of Knowledge and Strategies for Informing Future Research. Environ. Toxicol. Chem. 2021, 40 (3), 606– 630,  DOI: 10.1002/etc.4890
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      Per- and Polyfluoroalkyl Substance Toxicity and Human Health Review: Current State of Knowledge and Strategies for Informing Future Research
      Fenton, Suzanne E.; Ducatman, Alan; Boobis, Alan; DeWitt, Jamie C.; Lau, Christopher; Ng, Carla; Smith, James S.; Roberts, Stephen M.
      Environmental Toxicology and Chemistry (2021), 40 (3), 606-630CODEN: ETOCDK; ISSN:0730-7268. (Wiley-Blackwell)
      Reports of environmental and human health impacts of per- and polyfluoroalkyl substances (PFAS) have greatly increased in the peer-reviewed literature. The goals of the present review are to assess the state of the science regarding toxicol. effects of PFAS and to develop strategies for advancing knowledge on the health effects of this large family of chems. Currently, much of the toxicity data available for PFAS are for a handful of chems., primarily legacy PFAS such as perfluorooctanoic acid and perfluorooctane sulfonate. Epidemiol. studies have revealed assocns. between exposure to specific PFAS and a variety of health effects, including altered immune and thyroid function, liver disease, lipid and insulin dysregulation, kidney disease, adverse reproductive and developmental outcomes, and cancer. Concordance with exptl. animal data exists for many of these effects. However, information on modes of action and adverse outcome pathways must be expanded, and profound differences in PFAS toxicokinetic properties must be considered in understanding differences in responses between the sexes and among species and life stages. With many health effects noted for a relatively few example compds. and hundreds of other PFAS in commerce lacking toxicity data, more contemporary and high-throughput approaches such as read-across, mol. dynamics, and protein modeling are proposed to accelerate the development of toxicity information on emerging and legacy PFAS, individually and as mixts. In addn., an appropriate degree of precaution, given what is already known from the PFAS examples noted, may be needed to protect human health. Environ Toxicol Chem 2020;00:1-25. 2020 SETAC.
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    13. 13
      Rappazzo, K. M.; Coffman, E.; Hines, E. P. Exposure to Perfluorinated Alkyl Substances and Health Outcomes in Children: A Systematic Review of the Epidemiologic Literature. Int. J. Environ. Res. Public Health 2017, 14 (7), 691,  DOI: 10.3390/ijerph14070691
      13
      Exposure to perfluorinated alkyl substances and health outcomes in children: a systematic review of the epidemiologic literature
      Rappazzo, Kristen M.; Coffman, Evan; Hines, Erin P.
      International Journal of Environmental Research and Public Health (2017), 14 (7), 691/1-691/22CODEN: IJERGQ; ISSN:1660-4601. (MDPI AG)
      Perfluoroalkyl substances (PFAS), chems. used to make products stain and stick resistant, have been linked to health effects in adults and adverse birth outcomes. A growing body of literature also addresses health effects in children exposed to PFAS. This review summarizes the epidemiol. evidence for relationships between prenatal and/or childhood exposure to PFAS and health outcomes in children as well as to provide a risk of bias anal. of the literature. A systematic review was performed by searching PubMed for studies on PFAS and child health outcomes. We identified 64 studies for inclusion and performed risk of bias anal. on those studies. We detd. that risk of bias across studies was low to moderate. Six categories of health outcomes emerged. These were: immunity/infection/asthma, cardio-metabolic, neurodevelopmental/attention, thyroid, renal, and puberty onset. While there are a limited no. of studies for any one particular health outcome, there is evidence for pos. assocns. between PFAS and dyslipidemia, immunity (including vaccine response and asthma), renal function, and age at menarche. One finding of note is that while PFASs are mixts. of multiple compds. few studies examine them as such, therefore the role of these compds. as complex mixts. remains largely unknown.
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    14. 14
      Xiao, C.; Grandjean, P.; Valvi, D.; Nielsen, F.; Jensen, T. K.; Weihe, P.; Oulhote, Y. Associations of Exposure to Perfluoroalkyl Substances with Thyroid Hormone Concentrations and Birth Size. J. Clin. Endocrinol. Metab 2019, 735,  DOI: 10.1210/clinem/dgz147
      There is no corresponding record for this reference.
    15. 15
      Lin, P.-I. D.; Cardenas, A.; Hauser, R.; Gold, D. R.; Kleinman, K. P.; Hivert, M.-F.; Fleisch, A. F.; Calafat, A. M.; Webster, T. F.; Horton, E. S.; Oken, E. Per- and Polyfluoroalkyl Substances and Blood Lipid Levels in Pre-Diabetic Adults-Longitudinal Analysis of the Diabetes Prevention Program Outcomes Study. Environ. Int. 2019, 129, 343– 353,  DOI: 10.1016/j.envint.2019.05.027
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      Per- and polyfluoroalkyl substances and blood lipid levels in pre-diabetic adults-longitudinal analysis of the diabetes prevention program outcomes study
      Lin, Pi-I. D.; Cardenas, Andres; Hauser, Russ; Gold, Diane R.; Kleinman, Ken P.; Hivert, Marie-France; Fleisch, Abby F.; Calafat, Antonia M.; Webster, Thomas F.; Horton, Edward S.; Oken, Emily
      Environment International (2019), 129 (), 343-353CODEN: ENVIDV; ISSN:0160-4120. (Elsevier Ltd.)
      We examd. the relationship of baseline plasma PFAS concns. with repeated measures of blood lipids. We included 888 prediabetic adults from the Diabetes Prevention Program (DPP) and DPP Outcomes Study, who had measurements of 6 plasma PFAS concns. at baseline (1996-1999) and repeated measures of blood lipids over 15 years of follow-up, and were initially randomized to placebo or a lifestyle intervention. Participants (65.9% female, 57.0% White, 65.9% aged 40-59 years) had comparable PFAS concns. [e.g., median (IQR) perfluorooctanoic acid (PFOA) 4.9 ng/mL (3.2)] with the general U. S. population in 1999-2000. We obsd. higher total cholesterol at baseline per doubling of PFOA (β: 6.1 mg/dL, 95% CI: 3.1, 9.04), perfluorohexane sulfonic acid (PFHxS, β: 2.2 mg/dL, 95% CI: 0.2, 4.3), and perfluorononanoic acid (PFNA, β: 2.9 mg/dL, 95% CI: 0.7, 5.0). Prospectively, baseline concns. of several PFASs, including PFOA, PFOS, PFHxS and PFNA, predicted higher risks of incident hypercholesterolemia and hypertriglyceridemia, but only in the placebo group and not the lifestyle intervention group. For example, participants in the placebo group with PFOA concn. > median (4.9 ng/mL) were almost twice as likely (HR: 1.90, 95% CI: 1.25, 2.88) to develop hypertriglyceridemia compared to those ≤median. Findings suggest adverse effects of some PFASs on lipid profiles in prediabetic adults. However, the detrimental effect was attenuated with a lifestyle intervention.
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    16. 16
      Liew, Z.; Goudarzi, H.; Oulhote, Y. Developmental Exposures to Perfluoroalkyl Substances (PFASs): An Update of Associated Health Outcomes. Curr. Environ. Heal. reports 2018, 5 (1), 1– 19,  DOI: 10.1007/s40572-018-0173-4
      16
      Developmental Exposures to Perfluoroalkyl Substances (PFASs): An Update of Associated Health Outcomes
      Liew, Zeyan; Goudarzi, Houman; Oulhote, Youssef
      Current Environmental Health Reports (2018), 5 (1), 1-19CODEN: CEHRB3; ISSN:2196-5412. (Springer International Publishing AG)
      Purpose of Review: We reviewed and summarized the epidemiol. evidence for the influence that pre- and postnatal exposures to perfluoroalkyl substances (PFASs) may have on health outcomes in offspring, with a particular focus on birth outcomes and postnatal growth, immunomodulatory effects and neurodevelopment. Recent Findings: PFASs are persistent org. pollutants that have been widely produced and used in a range of com. products since the 1950s. Human exposures to PFASs are nearly ubiquitous globally, but studies that addressed potential health effects of PFASs have only begun to accumulate in recent years. Animal studies suggest adverse effects resulting from developmental encompasses prenatal exposures to PFASs. In humans, the developing fetus is exposed to PFASs via active or passive placenta transfer, while newborns might be exposed via breastfeeding or PFAS in the home environment. Summary: Overall, epidemiol. findings are consistent and suggest possible assocns. with fetal and postnatal growth and immune function, while the findings on neurodevelopmental endpoints to date are rather inconclusive. Methodol. challenges and future directions for PFASs-focused research are discussed.
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    17. 17
      Barry, V.; Winquist, A.; Steenland, K. Perfluorooctanoic Acid (PFOA) Exposures and Incident Cancers among Adults Living near a Chemical Plant. Environ. Health Perspect 2013, 121 (11–12), 1313– 1318,  DOI: 10.1289/ehp.1306615
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      Perfluorooctanoic acid (PFOA) exposures and incident cancers among adults living near a chemical plant
      Barry Vaughn; Winquist Andrea; Steenland Kyle
      Environmental health perspectives (2013), 121 (11-12), 1313-8 ISSN:.
      BACKGROUND: Perfluorooctanoic acid (PFOA) is a synthetic chemical ubiquitous in the serum of U.S. residents. It causes liver, testicular, and pancreatic tumors in rats. Human studies are sparse. OBJECTIVE: We examined cancer incidence in Mid-Ohio Valley residents exposed to PFOA in drinking water due to chemical plant emissions. METHODS: The cohort consisted of adult community residents who resided in contaminated water districts or worked at a local chemical plant. Most participated in a 2005-2006 baseline survey in which serum PFOA was measured. We interviewed the cohort in 2008-2011 to obtain further medical history. Retrospective yearly PFOA serum concentrations were estimated for each participant from 1952 through 2011. Self-reported cancers were validated through medical records and cancer registry review. We estimated the association between cancer and cumulative PFOA serum concentration using proportional hazards models. RESULTS: Participants (n = 32,254) reported 2,507 validated cancers (21 different cancer types). Estimated cumulative serum PFOA concentrations were positively associated with kidney and testicular cancer [hazard ratio (HR) = 1.10; 95% CI: 0.98, 1.24 and HR = 1.34; 95% CI: 1.00, 1.79, respectively, for 1-unit increases in ln-transformed serum PFOA]. Categorical analyses also indicated positive trends with increasing exposures for both cancers: for kidney cancer HRs for increasing exposure quartiles were 1.0, 1.23, 1.48, and 1.58 (linear trend test p = 0.18) and for testicular cancer, HRs were 1.0, 1.04, 1.91, 3.17 (linear trend test p = 0.04). CONCLUSIONS: PFOA exposure was associated with kidney and testicular cancer in this population. Because this is largely a survivor cohort, findings must be interpreted with caution, especially for highly fatal cancers such as pancreatic and lung cancer.
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    18. 18
      Stanifer, J. W.; Stapleton, H. M.; Souma, T.; Wittmer, A.; Zhao, X.; Boulware, L. E. Perfluorinated Chemicals as Emerging Environmental Threats to Kidney Health: A Scoping Review. Clin. J. Am. Soc. Nephrol 2018, 13 (10), 1479– 1492,  DOI: 10.2215/CJN.04670418
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      Perfluorinated chemicals as emerging environmental threats to kidney health: a scoping review
      Stanifer, John W.; Stapleton, Heather M.; Souma, Tomokazu; Wittmer, Ashley; Zhao, Xinlu; Boulware, L. Ebony
      Clinical Journal of the American Society of Nephrology (2018), 13 (10), 1479-1492CODEN: CJASC7; ISSN:1555-9041. (American Society of Nephrology)
      Background and objectives Per- and polyfluoroalkyl substances (PFASs) are a large group of manufd. nonbiodegradable compds. Despite increasing awareness as global pollutants, the impact of PFAS exposure on human health is not well understood, and there are growing concerns for adverse effects on kidney function. Therefore, we conducted a scoping review to summarize and identify gaps in the understanding between PFAS exposure and kidney health. Design, setting, participants, & measurements We systematically searched PubMed, EMBASE, EBSCO Global Health, World Health Organization Global Index, and Web of Science for studies published from 1990 to 2018. We included studies on the epidemiol., pharmacokinetics, or toxicol. of PFAS exposure and kidney-related health, including clin., histol., mol., and metabolic outcomes related to kidney disease, or outcomes related to the pharmacokinetic role of the kidneys. Results We identified 74 studies, including 21 epidemiol., 13 pharmacokinetic, and 40 toxicol. studies. Three population-based epidemiol. studies demonstrated assocns. between PFAS exposure and lower kidney function. Along with toxicol. studies (n = 10) showing tubular histol. and cellular changes from PFAS exposure, pharmacokinetic studies (n=5) demonstrated the kidneys were major routes of elimination, with active proximal tubule transport.
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    19. 19
      Young, A. S.; Hauser, R.; James-Todd, T. M.; Coull, B. A.; Zhu, H.; Kannan, K.; Specht, A. J.; Bliss, M. S.; Allen, J. G. Impact of “Healthier” Materials Interventions on Dust Concentrations of per- and Polyfluoroalkyl Substances, Polybrominated Diphenyl Ethers, and Organophosphate Esters. Environ. Int. 2021, 150, 106151,  DOI: 10.1016/j.envint.2020.106151
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      Impact of "healthier" materials interventions on dust concentrations of per- and polyfluoroalkyl substances, polybrominated diphenyl ethers, and organophosphate esters
      Young, Anna S.; Hauser, Russ; James-Todd, Tamarra M.; Coull, Brent A.; Zhu, Hongkai; Kannan, Kurunthachalam; Specht, Aaron J.; Bliss, Maya S.; Allen, Joseph G.
      Environment International (2021), 150 (), 106151CODEN: ENVIDV; ISSN:0160-4120. (Elsevier Ltd.)
      Per- and polyfluoroalkyl substances (PFAS), polybrominated di-Ph ethers (PBDEs), and organophosphate esters (OPEs) are found in building materials and assocd. with thyroid disease, infertility, and impaired development. We measured 15 PFAS, 8 PBDEs, and 19 OPEs in dust from offices, common areas, and class rooms having undergone either no intervention (conventional rooms in older buildings meeting strict fire codes; n = 12), full "healthier" materials interventions (rooms with "healthier" materials in buildings constructed more recently or gut-renovated; n = 7), or partial interventions (other rooms with at least "healthier" foam furniture but more potential building contamination; n = 28). In multilevel regression models, rooms with full "healthier" materials interventions had 78% lower dust levels of PFAS. Rooms with full "healthier" interventions also had 65% lower OPE levels in dust than rooms with no intervention (p < 0.01) and 45% lower PBDEs than rooms with only partial interventions (p< 0.10), adjusted for covariates related to insulation, electronics, and furniture. Bromine loadings from electronics in rooms were assocd. with PBDE concns. in dust (p < 0.05), and the presence of exposed insulation was assocd. with OPE dust concns. (p < 0.001). Full "healthier" materials renovations successfully reduced chem. classes in dust. Future interventions should address electronics, insulation, and building cross-contamination.
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    20. 20
      Miyake, Y.; Yamashita, N.; So, M. K.; Rostkowski, P.; Taniyasu, S.; Lam, P. K. S.; Kannan, K. Trace Analysis of Total Fluorine in Human Blood Using Combustion Ion Chromatography for Fluorine: A Mass Balance Approach for the Determination of Known and Unknown Organofluorine Compounds. J. Chromatogr. A 2007, 1154 (1–2), 214– 221,  DOI: 10.1016/j.chroma.2007.03.084
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      Trace analysis of total fluorine in human blood using combustion ion chromatography for fluorine: A mass balance approach for the determination of known and unknown organofluorine compounds
      Miyake, Yuichi; Yamashita, Nobuyoshi; So, Man Ka; Rostkowski, Pawel; Taniyasu, Sachi; Lam, Paul K. S.; Kannan, Kurunthachalam
      Journal of Chromatography A (2007), 1154 (1-2), 214-221CODEN: JCRAEY; ISSN:0021-9673. (Elsevier B.V.)
      The no. of perfluorochems. (PFCs) that have been found in biol. and environmental matrixes is increasing as anal. stds. and methods evolve. Perfluorooctanesulfonate (PFOS) and perfluorooctanoate (PFOA) constitute only a fraction of the total suite of PFCs found in environmental and biol. matrixes. A robust method and approach is needed to evaluate the mass of fluorinated compds. in biol. matrixes. In this study, we developed a method to measure total fluorine (TF) and org. fluorine (TOF) in human blood matrixes using combustion ion chromatog. (CIC). Blood matrixes (whole blood, serum, and plasma) were analyzed in bulk to det. TF. An aliquot of the blood was also extd. with org. solvents such as methyl-tert-Bu ether (MTBE) and hexane, and org. and aq. exts. were sepd., to fractionate organofluorines from inorg. fluorine. The org. layer was analyzed for TF by CIC, and for known PFCs by high performance liq. chromatog.-tandem mass spectrometry (HPLC-MS/MS). PFCs measured by HPLC-MS/MS accounted for >80% of the TF in the org. fraction. The aq. fraction contained inorg. fluorine and other non-extractable organofluorines. However, in the bulk sample, fluoride and non-extractable organofluorines accounted for >70% of the TF in blood samples from the general population. In occupationally exposed individuals, known organofluorines accounted for a major proportion of the TF. These results suggest the existence of yet uncharacterized fluorine fraction in human blood. Further studies are needed to characterize the aq. fraction that contains inorg. fluorine and non-extractable forms of fluorine.
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    21. 21
      Ritter, E. E.; Dickinson, M. E.; Harron, J. P.; Lunderberg, D. M.; DeYoung, P. A.; Robel, A. E.; Field, J. A.; Peaslee, G. F. PIGE as a Screening Tool for Per- and Polyfluorinated Substances in Papers and Textiles. Nucl. Instruments Methods Phys. Res. Sect. B Beam Interact. with Mater. Atoms 2017, 407, 47– 54,  DOI: 10.1016/j.nimb.2017.05.052
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      PIGE as a screening tool for Per- and polyfluorinated substances in papers and textiles
      Ritter, Evelyn E.; Dickinson, Margaret E.; Harron, John P.; Lunderberg, David M.; DeYoung, Paul A.; Robel, Alix E.; Field, Jennifer A.; Peaslee, Graham F.
      Nuclear Instruments & Methods in Physics Research, Section B: Beam Interactions with Materials and Atoms (2017), 407 (), 47-54CODEN: NIMBEU; ISSN:0168-583X. (Elsevier B.V.)
      Per- and polyfluoroalkyl substances (PFASs) comprise a large array of man-made fluorinated chems. It is an emerging chem. class of concern because many PFASs are environmentally persistent and some have known ecol. and human toxicity. Consumer products treated with PFASs result in human exposure to PFASs through inhalation, ingestion, and environmental exposure to emissions from wastewater or from landfills. A rapid screening method based on total fluorine was developed and applied to quantify PFASs on consumer papers and textiles. Particle-Induced Gamma Ray Emission (PIGE) spectroscopy provides a non-destructive and quant. measurement of total fluorine on papers and textiles. This technique is both rapid and sensitive, with a limit of detection (LOD) of 13 nmol F/cm2 for papers and 24-45 nmol F/cm2 for textiles, with reproducibility of ±12% RSD for both. PIGE is a high throughput (>20 samples/h typically) method that was applied to 50 papers and 50 textiles in commerce to demonstrate the method.
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    22. 22
      Schultes, L.; Peaslee, G. F.; Brockman, J. D.; Majumdar, A.; McGuinness, S. R.; Wilkinson, J. T.; Sandblom, O.; Ngwenyama, R. A.; Benskin, J. P. Total Fluorine Measurements in Food Packaging: How Do Current Methods Perform?. Environ. Sci. Technol. Lett. 2019, 6 (2), 73– 78,  DOI: 10.1021/acs.estlett.8b00700
      22
      Total fluorine measurements in food packaging: How do current methods perform?
      Schultes, Lara; Peaslee, Graham F.; Brockman, John D.; Majumdar, Ashabari; McGuinness, Sean R.; Wilkinson, John T.; Sandblom, Oskar; Ngwenyama, Ruth A.; Benskin, Jonathan P.
      Environmental Science & Technology Letters (2019), 6 (2), 73-78CODEN: ESTLCU; ISSN:2328-8930. (American Chemical Society)
      Per- and polyfluoroalkyl substances (PFASs) represent a class of more than 4000 compds. Their large no. and structural diversity pose a considerable challenge to anal. chemists. Measurement of total fluorine in environmental samples and consumer products is therefore crit. for rapidly screening for PFASs and for assessing the fraction of unexplained fluorine(i.e., fluorine mass balance). Here we compare three emerging anal. techniques for total fluorine detn.: combustion ion chromatog. (CIC), particle-induced γ-ray emission spectroscopy (PIGE), and instrumental neutron activation anal. (INAA). Application of each method to a certified ref. material (CRM), spiked filters, and representative food packaging samples revealed good accuracy and precision. INAA and PIGE had the advantage of being nondestructive, while CIC displayed the lowest detection limits. Inconsistencies between the methods arose due to the high aluminum content in the CRM, which precluded its anal. by INAA, and sample heterogeneity (i.e., coating on the surface of the material), which resulted in higher values from the surface measurement technique PIGE compared to the values from the bulk vol. techniques INAA and CIC. Comparing CIC-based extractable org. fluorine to target PFAS measurements of food packaging samples by liq. chromatog.-tandem mass spectrometry revealed large amts. of unidentified org. fluorine not captured by compd.-specific anal.
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    23. 23
      De Silva, A. O.; Armitage, J. M.; Bruton, T. A.; Dassuncao, C.; Heiger-Bernays, W.; Hu, X. C.; Kärrman, A.; Kelly, B.; Ng, C.; Robuck, A.; Sun, M.; Webster, T. F.; Sunderland, E. M. PFAS Exposure Pathways for Humans and Wildlife: A Synthesis of Current Knowledge and Key Gaps in Understanding. Environ. Toxicol. Chem. 2021, 40 (3), 631– 657,  DOI: 10.1002/etc.4935
      23
      PFAS Exposure Pathways for Humans and Wildlife: A Synthesis of Current Knowledge and Key Gaps in Understanding
      De Silva, Amila O.; Armitage, James M.; Bruton, Thomas A.; Dassuncao, Clifton; Heiger-Bernays, Wendy; Hu, Xindi C.; Kaerrman, Anna; Kelly, Barry; Ng, Carla; Robuck, Anna; Sun, Mei; Webster, Thomas F.; Sunderland, Elsie M.
      Environmental Toxicology and Chemistry (2021), 40 (3), 631-657CODEN: ETOCDK; ISSN:0730-7268. (Wiley-Blackwell)
      A review. We synthesize current understanding of the magnitudes and methods for assessing human and wildlife exposures to poly- and perfluoroalkyl substances (PFAS). Most human exposure assessments have focused on 2 to 5 legacy PFAS, and wildlife assessments are typically limited to targeted PFAS (up to ∼30 substances). However, shifts in chem. prodn. are occurring rapidly, and targeted methods for detecting PFAS have not kept pace with these changes. Total fluorine measurements complemented by suspect screening using high-resoln. mass spectrometry are thus emerging as essential tools for PFAS exposure assessment. Such methods enable researchers to better understand contributions from precursor compds. that degrade into terminal perfluoroalkyl acids. Available data suggest that diet is the major human exposure pathway for some PFAS, but there is large variability across populations and PFAS compds. Addnl. data on total fluorine in exposure media and the fraction of unidentified organofluorine are needed. Drinking water has been established as the major exposure source in contaminated communities. As water supplies are remediated, for the general population, exposures from dust, personal care products, indoor environments, and other sources may be more important. A major challenge for exposure assessments is the lack of statistically representative population surveys. For wildlife, bioaccumulation processes differ substantially between PFAS and neutral lipophilic org. compds., prompting a reevaluation of traditional bioaccumulation metrics. There is evidence that both phospholipids and proteins are important for the tissue partitioning and accumulation of PFAS. New mechanistic models for PFAS bioaccumulation are being developed that will assist in wildlife risk evaluations.
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    24. 24
      Robel, A. E.; Marshall, K.; Dickinson, M.; Lunderberg, D.; Butt, C.; Peaslee, G.; Stapleton, H. M.; Field, J. A. Closing the Mass Balance on Fluorine on Papers and Textiles. Environ. Sci. Technol. 2017, 51 (16), 9022– 9032,  DOI: 10.1021/acs.est.7b02080
      24
      Closing the Mass Balance on Fluorine on Papers and Textiles
      Robel, Alix E.; Marshall, Kristin; Dickinson, Margaret; Lunderberg, David; Butt, Craig; Peaslee, Graham; Stapleton, Heather M.; Field, Jennifer A.
      Environmental Science & Technology (2017), 51 (16), 9022-9032CODEN: ESTHAG; ISSN:0013-936X. (American Chemical Society)
      Paper and textiles treated with per- and polyfluoroalkyl substances (PFAS) are sources of human and environmental exposure. Data for individual PFAS, e.g., perfluorooctanesulfonate (PFOS) and perfluorooctanoate (PFOA), are not placed in the context of total F for paper and textiles. Gas chromatog./mass spectrometry (GC/MS) and liq. chromatog./tandem mass spectrometry (LC/MS-MS) quantified volatile and ionic PFAS, resp.; the total oxidizable precursor (TOP) assay quantified precursors which form perfluoroalkyl carboxylates. Molar sums of PFAS obtained by GC/MS, LC/MS-/MS, and precursors were compared to total F (nmol F/cm2) detd. by particle-induced gamma ray emission (PIGE) spectroscopy, measured before and after extn. Volatile and ionic PFAS and unknown precursors accounted for 0-2.2%, 0-0.41%, and 0.021-14%, resp., of total nmol F/cm2 detd. by PIGE. Following extn., paper and textiles retained 64 ± 28% to 110 ± 30% of the original nmol F/cm2 as detd. by PIGE, indicating the majority of F remains assocd. with the paper and textiles. The sum of PFAS in volatile, ionic, and precursor fractions, and total F post-extn. indicated that mass balance was achieved (within anal. error) of the initial total F measured by PIGE.
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    25. 25
      Schultes, L.; Vestergren, R.; Volkova, K.; Westberg, E.; Jacobson, T.; Benskin, J. P. Per- and Polyfluoroalkyl Substances and Fluorine Mass Balance in Cosmetic Products from the Swedish Market: Implications for Environmental Emissions and Human Exposure. Environ. Sci. Process. Impacts 2018, 20 (12), 1680– 1690,  DOI: 10.1039/C8EM00368H
      25
      Per- and polyfluoroalkyl substances and fluorine mass balance in cosmetic products from the Swedish market: implications for environmental emissions and human exposure
      Schultes, Lara; Vestergren, Robin; Volkova, Kristina; Westberg, Emelie; Jacobson, Therese; Benskin, Jonathan P.
      Environmental Science: Processes & Impacts (2018), 20 (12), 1680-1690CODEN: ESPICZ; ISSN:2050-7895. (Royal Society of Chemistry)
      Per-and polyfluoroalkyl substances (PFASs) are a diverse class of < 4700 chems. used in com. products and industrial processes. Concerns surrounding PFASs are principally due to their widespread occurrence in humans and the environment and links to adverse health effects. One of the lesser known uses for PFASs is in cosmetic products (CPs) which come into contact with the skin (e.g. hair products, powders, sunblocks, etc.). In the present work, thirty-one CPs from five product categories (cream, foundation, pencil, powder and shaving foam) were analyzed for 39 PFASs by liq. chromatog.-tandem mass spectrometry, as well as extractable org. fluorine (EOF) and total fluorine (TF) by combustion ion chromatog. (CIC). This multi-platform approach enabled detn. of the fraction of fluorine accounted for by known PFASs (i.e. fluorine mass balance). Foundations and powders contained 25 different PFASs with the most frequently detected being perfluorinated carboxylic acids (perfluoroheptanoic acid and perfluorohexanoic acid) and polyfluoroalkyl phosphate esters (PAPs). U+03C314PAP concns. up to 470μg g-1 were measured in products listing mixts. of PAPs as an ingredient. For all samples, U+03C3 39PFAS concns. only explained a small fraction of the EOF and TF, pointing to the presence of unknown org. and/or inorg. fluorinated substances, including polymers. While creams, pencil and shaving foams did not contain measurable concns. of any of the 39 PFASs targeted here, CIC revealed high to moderate TF content. Overall, these data highlight the need for further investigations into the occurrence of PFASs in CPs and their importance with regards to human and environmental exposure.
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    26. 26
      Peaslee, G. F.; Wilkinson, J. T.; McGuinness, S. R.; Tighe, M.; Caterisano, N.; Lee, S.; Gonzales, A.; Roddy, M.; Mills, S.; Mitchell, K. Another Pathway for Firefighter Exposure to Per- and Polyfluoroalkyl Substances: Firefighter Textiles. Environ. Sci. Technol. Lett. 2020, 7 (8), 594– 599,  DOI: 10.1021/acs.estlett.0c00410
      26
      Another Pathway for Firefighter Exposure to Per- and Polyfluoroalkyl Substances: Firefighter Textiles
      Peaslee, Graham F.; Wilkinson, John T.; McGuinness, Sean R.; Tighe, Meghanne; Caterisano, Nicholas; Lee, Seryeong; Gonzales, Alec; Roddy, Matthew; Mills, Simon; Mitchell, Krystle
      Environmental Science & Technology Letters (2020), 7 (8), 594-599CODEN: ESTLCU; ISSN:2328-8930. (American Chemical Society)
      Occupational exposure to aq. film-forming foams (AFFF) can lead to elevated concns. of per- and polyfluorinated alkyl substances (PFAS) in firefighter blood sera. AFFF are also one PFAS exposure source in the general population due to their environmental persistence and soly. in groundwater. Due to documented PFAS adverse health effects, the primary concern to date for the fire services centered on repeated AFFF use and exposure. This work presents an addnl. PFAS exposure source for firefighters: PFAS shed from their protective clothing. Textiles in firefighter turn-out gear had high total F concns. (up to 2%); individual PFAS were identified and measured on new and used firefighting turn-out gear. Used gear showed lower PFAS concn. and increased migration to untreated material. Textile storage area dust measurements also suggested direct loss of PFAS from the textile fluoropolymers. Since PFAS shed from turn-out gear textiles are more mobile, they represent another exposure source for firefighters which warrants addnl. study.
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    27. 27
      Tokranov, A. K.; Nishizawa, N.; Amadei, C. A.; Zenobio, J. E.; Pickard, H. M.; Allen, J. G.; Vecitis, C. D.; Sunderland, E. M. How Do We Measure Poly- and Perfluoroalkyl Substances (PFASs) at the Surface of Consumer Products?. Environ. Sci. Technol. Lett. 2018, 6, 38,  DOI: 10.1021/acs.estlett.8b00600
      There is no corresponding record for this reference.
    28. 28
      Poothong, S.; Papadopoulou, E.; Padilla-Sánchez, J. A.; Thomsen, C.; Haug, L. S. Multiple Pathways of Human Exposure to Poly- and Perfluoroalkyl Substances (PFASs): From External Exposure to Human Blood. Environ. Int. 2020, 134, 105244,  DOI: 10.1016/j.envint.2019.105244
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      Multiple pathways of human exposure to poly- and perfluoroalkyl substances (PFASs): From external exposure to human blood
      Poothong, Somrutai; Papadopoulou, Eleni; Padilla-Sanchez, Juan Antonio; Thomsen, Cathrine; Haug, Line Smaastuen
      Environment International (2020), 134 (), 105244CODEN: ENVIDV; ISSN:0160-4120. (Elsevier Ltd.)
      This study aimed to characterize the exposure to PFASs from diet, house dust, indoor air, and dermal contact and the relative contribution from different external exposure pathways to human serum concns. Concns. of PFAAs and PFAA precursors in house dust, indoor air, hand wipes, foods and drinks were utilized to est. the daily intakes. Dietary exposure from ingestion of food and drinks was in general the predominant exposure pathway, followed by exposure from ingestion of house dust, inhalation of indoor air, and dermal absorption, but considerable variations were obsd. among individuals. House dust ingestion and indoor air inhalation contributed most to the total intakes for some participants, for which most of them were among the 20% participants with the highest total estd. intakes. Some statistical significant assocns. between concns. of PFASs measured in serum and estd. intakes were obsd. Measured serum concns. and modelled serum concns. based on external exposure ests. were in the same order of magnitude for PFOS, PFHxS, PFOA, and PFNA, but only PFOA concns. were comparable, 1.9 and 2.0 ng mL-1 for obsd. and modelled serum concns., resp. The estd. daily intakes of PFASs in this study were lower than the health-based guidance values, e.g. the tolerable weekly intakes derived by EFSA. This study underlines the importance of performing studies considering multiple exposure pathways on an individual basis.
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    29. 29
      Mitro, S. D.; Dodson, R. E.; Singla, V.; Adamkiewicz, G.; Elmi, A. F.; Tilly, M. K.; Zota, A. R. Consumer Product Chemicals in Indoor Dust: A Quantitative Meta-Analysis of U.S. Studies. Environ. Sci. Technol. 2016, 50 (19), 10661– 10672,  DOI: 10.1021/acs.est.6b02023
      29
      Consumer Product Chemicals in Indoor Dust: A Quantitative Meta-analysis of U.S. Studies
      Mitro, Susanna D.; Dodson, Robin E.; Singla, Veena; Adamkiewicz, Gary; Elmi, Angelo F.; Tilly, Monica K.; Zota, Ami R.
      Environmental Science & Technology (2016), 50 (19), 10661-10672CODEN: ESTHAG; ISSN:0013-936X. (American Chemical Society)
      Indoor dust is a reservoir for com. consumer product chems., including many compds. with known or suspected health effects; however, most dust exposure studies measure few chems. in small samples. This work systematically searched the US indoor dust literature on phthalates, replacement flame retardants (RFR), perfluoroalkyl substances (PFAS), synthetic fragrances, and environmental phenols, and estd. pooled geometric means (GM) and 95% confidence intervals for 45 chems. measured in ≥3 datasets. Pooled GM calcd. residential intake from dust ingestion, inhalation, and dermal uptake from air, then hazard traits from the Safer Consumer Products Candidate Chem. List were identified to rank and contextualize these results. Results indicated US indoor dust consistently contains chems. from multiple classes. Phthalates occurred in the highest concns., followed by phenols, RFR, fragrance, and PFAS; several phthalates and RFR had the highest residential intakes. Many chems. in dust share hazard traits, e.g., reproductive and endocrine toxicity. Recommendations are made to maximize study comparability and advance indoor exposure science. This information is crit. in shaping future exposure and health studies, particularly related to cumulative exposure, and providing evidence for intervention development and public policy.
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    30. 30
      Ruyle, B. J.; Pickard, H. M.; LeBlanc, D. R.; Tokranov, A. K.; Thackray, C. P.; Hu, X. C.; Vecitis, C. D.; Sunderland, E. M. Isolating the AFFF Signature in Coastal Watersheds Using Oxidizable PFAS Precursors and Unexplained Organofluorine. Environ. Sci. Technol. 2021, 55 (6), 3686– 3695,  DOI: 10.1021/acs.est.0c07296
      30
      Isolating the AFFF signature in coastal watersheds using oxidizable PFAS precursors and unexplained organofluorine
      Ruyle, Bridger J.; Pickard, Heidi M.; LeBlanc, Denis R.; Tokranov, Andrea K.; Thackray, Colin P.; Hu, Xindi C.; Vecitis, Chad D.; Sunderland, Elsie M.
      Environmental Science & Technology (2021), 55 (6), 3686-3695CODEN: ESTHAG; ISSN:0013-936X. (American Chemical Society)
      Water supplies for millions of U.S. individuals exceed max. contaminant levels for per- and polyfluoroalkyl substances (PFAS). Contemporary and legacy use of aq. film forming foams (AFFF) is a major contamination source. However, diverse PFAS sources are present within watersheds, making it difficult to isolate their predominant origins. Here we examine PFAS source signatures among six adjacent coastal watersheds on Cape Cod, MA, U.S.A. using multivariate clustering techniques. A distinct signature of AFFF contamination enriched in precursors with six perfluorinated carbons (C6) was identified in watersheds with an AFFF source, while others were enriched in C4 precursors. Principal component anal. of PFAS compn. in impacted watersheds showed a decline in precursor compn. relative to AFFF stocks and a corresponding increase in terminal perfluoroalkyl sulfonates with < C6 but not those with ≥ C6. Prior work shows that in AFFF stocks, all extractable organofluorine (EOF) can be explained by targeted PFAS and precursors inferred using Bayesian inference on the total oxidizable precursor assay. Using the same techniques for the first time in impacted watersheds, we find that only 24%-63% of the EOF can be explained by targeted PFAS and oxidizable precursors. Our work thus indicates the presence of large non-AFFF organofluorine sources in these coastal watersheds.
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    31. 31
      Young, A. S.; Sparer-Fine, E. H.; Pickard, H. M.; Sunderland, E. M.; Peaslee, G. F.; Allen, J. G. Per- and Polyfluoroalkyl Substances (PFAS) and Total Fluorine in Fire Station Dust. J. Expo. Sci. Environ. Epidemiol 2021, 930,  DOI: 10.1038/s41370-021-00288-7
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      Per- and polyfluoroalkyl substances (PFAS) and total fluorine in fire station dust
      Young, Anna S.; Sparer-Fine, Emily H.; Pickard, Heidi M.; Sunderland, Elsie M.; Peaslee, Graham F.; Allen, Joseph G.
      Journal of Exposure Science & Environmental Epidemiology (2021), 31 (5), 930-942CODEN: JESEBS; ISSN:1559-0631. (Nature Portfolio)
      Abstr.: Per- and polyfluoroalkyl substances (PFAS) are a class of over 4700 fluorinated compds. used in industry and consumer products. Studies have highlighted the use of aq. film-forming foams (AFFFs) as an exposure source for firefighters, but little is known about PFAS occurrence inside fire stations, where firefighters spend most of their shifts. In this study, we aimed to characterize PFAS concns. and sources inside fire stations. We measured 24 PFAS (using LC-MS/MS) and total fluorine (using particle-induced gamma ray emission) in dust from multiple rooms of 15 Massachusetts stations, many of which (60%) no longer use PFAS-contg. AFFF at all and the rest of which only use it very rarely. Compared to station living rooms, turnout gear locker rooms had higher dust levels of total fluorine (p < 0.0001) and three PFAS: perfluorohexanoate (PFHxA), perfluoroheptanoate (PFHpA), and perfluorodecanoate (PFDoDA) (p < 0.05). These PFAS were also found on six wipes of station turnout gear. By contrast, the dominant PFAS in living rooms was N-Et perfluorooctane sulfonamidoacetic acid (N-MeFOSAA), a precursor to perfluorooctane sulfonate (PFOS) that still persists despite phase-outs almost two decades ago. The Σ24 PFAS accounted for less than 2% of fluorine in dust (n = 39), suggesting the potential presence of unknown PFAS. Turnout gear may be an important PFAS source in stations due to intentional additives and/or contamination from firefighting activities.
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    32. 32
      Aro, R.; Carlsson, P.; Vogelsang, C.; Kärrman, A.; Yeung, L. W. Y. Fluorine Mass Balance Analysis of Selected Environmental Samples from Norway. Chemosphere 2021, 283, 131200,  DOI: 10.1016/j.chemosphere.2021.131200
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      Fluorine mass balance analysis of selected environmental samples from Norway
      Aro, Rudolf; Carlsson, Pernilla; Vogelsang, Christian; Kaerrman, Anna; Yeung, Leo WY.
      Chemosphere (2021), 283 (), 131200CODEN: CMSHAF; ISSN:0045-6535. (Elsevier Ltd.)
      The presence of unidentified organofluorine compds. (UOF) has been investigated in recent publication, but their environmental occurrence is still poorly understood. Fluorine mass balance anal. was performed on environmental samples from lake Mjosa and river Alna (surface water (n = 9), sediment (n = 5) and fish liver (n = 4)) and sewage samples from Oslo (n = 5), to reveal to the fraction of UOF. In samples that had extractable organofluorine (EOF) concns. above the limit of detection (LoD), more than 70% of their EOF could not be accounted for by the 37 PFAS monitored in this study. The surface water samples from lake Mjosa had EOF concns. several times higher than what has been reported elsewhere in Nordic nations. The flux of EOF in river Alna and selected sewage pipes revealed that it was 1-2 orders of magnitude higher than the flux of the measured PFAS. The elevated concns. of EOF in all samples pose a potential health and environmental hazard, as their compn. remains mostly unknown.
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    33. 33
      Yeung, L. W. Y.; Miyake, Y.; Li, P.; Taniyasu, S.; Kannan, K.; Guruge, K. S.; Lam, P. K. S.; Yamashita, N. Comparison of Total Fluorine, Extractable Organic Fluorine and Perfluorinated Compounds in the Blood of Wild and Pefluorooctanoate (PFOA)-Exposed Rats: Evidence for the Presence of Other Organofluorine Compounds. Anal. Chim. Acta 2009, 635 (1), 108– 114,  DOI: 10.1016/j.aca.2009.01.004
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      Comparison of total fluorine, extractable organic fluorine and perfluorinated compounds in the blood of wild and pefluorooctanoate (PFOA)-exposed rats: Evidence for the presence of other organofluorine compounds
      Yeung, Leo W. Y.; Miyake, Yuichi; Li, Peng; Taniyasu, Sachi; Kannan, Kurunthachalam; Guruge, Keerthi S.; Lam, Paul K. S.; Yamashita, Nobuyoshi
      Analytica Chimica Acta (2009), 635 (1), 108-114CODEN: ACACAM; ISSN:0003-2670. (Elsevier B.V.)
      The widespread occurrence and environmental persistence of perfluorinated compds. (PFCs) received worldwide attention recently. Exhaustive anal. of all fluorinated compds. in an environmental sample can be daunting because of the constraints in the availability of anal. stds. and extn. methods. Combustion ion chromatog. technique for trace fluorine anal. was used to assess the concns. of known PFCs (e.g., PFOS, PFOA) and total fluorine (TF) in the blood of wild rats collected from Japan. The technique was further validated using tissues from PFOA-exposed rats. Six PFCs (PFOS, PFOSA, PFUnDA, PFDA, PFNA, and PFOA) were detected in all of the wild rat blood samples. Concns. of extractable org. fluorine (EOF) in fraction 1 (Fr1; MTBE extn.) of wild rats ranged 60.9-134 ng F mL-1, while those in fraction 2 (Fr2; hexane) were below LOQ (32 ng F mL-1); TF concns. in the blood of wild rats ranged from 59.9-192 ng F mL-1. The contribution of known PFCs in EOF-Fr1 (MTBE) varied from 9% to 89% (56% on av.), and known PFC concns. in TF content were less than 25%. In contrast, TF concns. in the blood of PFOA-exposed rats ranged from 46900 to 111000 ng F mL-1, with PFOA contributing over 90% of TF. A comparison of results from the samples analyzed in this study and the literature revealed three distinct groups with PFOA/known PFC and TF levels (i.e., wild rats and general population, occupationally exposed workers, and PFOA-exposed lab. rats). The mass balance anal. of the different forms of fluorine in blood suggested the presence of other forms of org. fluorine in addn. to known PFCs.
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    34. 34
      Miyake, Y.; Yamashita, N.; Rostkowski, P.; So, M. K.; Taniyasu, S.; Lam, P. K. S.; Kannan, K. Determination of Trace Levels of Total Fluorine in Water Using Combustion Ion Chromatography for Fluorine: A Mass Balance Approach to Determine Individual Perfluorinated Chemicals in Water. J. Chromatogr. A 2007, 1143 (1–2), 98– 104,  DOI: 10.1016/j.chroma.2006.12.071
      34
      Determination of trace levels of total fluorine in water using combustion ion chromatography for fluorine: A mass balance approach to determine individual perfluorinated chemicals in water
      Miyake, Yuichi; Yamashita, Nobuyoshi; Rostkowski, Pawel; So, Man Ka; Taniyasu, Sachi; Lam, Paul K. S.; Kannan, Kurunthachalam
      Journal of Chromatography A (2007), 1143 (1-2), 98-104CODEN: JCRAEY; ISSN:0021-9673. (Elsevier B.V.)
      Perfluorinated compds. (PFC), e.g., perfluorooctanesulfonate (PFOS) and perfluorooctanoate (PFOA), have received worldwide attention due to their environmental persistence and widespread distribution. Due to a lack of robust anal. methods and stds. to detect all the PFC and their precursors and metabolic intermediates, a mass balance approach involving detn. of total F (TF), followed by sample fractionation sep. det. inorg. and org. F, is needed. This work developed a method to det. low μg/L concns. TF in seawater. Seawater samples were fractionated into org. and inorg. fractions by extn. with org. solvents, which were then analyzed for TF, extractable org. F (EOF) and inorg. F (IF, i.e., F-). Concns. of known perfluorinated compds. (PFC) including PFOS and PFOA were also detd. in water by liq. chromatog.-tandem mass spectrometry (LC-MS/MS) to calc. the fraction of F contributed by PFC to TF. A major proportion of F in seawater was in the form of F- (>90% at sites not affected by direct discharges). Nevertheless, within the organofluorine fraction, a major percentage (60-90%) of F still remains unknown in water samples, suggesting the occurrence of other fluorinated acids in addn. to known perfluorinated acids. Further studies are needed to identify and quantify unidentified organofluorines in seawater. Mass balance anal. of total org. F (TOF) and EOF is important, to understand fluorinated compd. environmental transport and fate and to identify sources of unidentified fluorinated compds.
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    35. 35
      Weber, A. K.; Barber, L. B.; LeBlanc, D. R.; Sunderland, E. M.; Vecitis, C. D. Geochemical and Hydrologic Factors Controlling Subsurface Transport of Poly- and Perfluoroalkyl Substances, Cape Cod, Massachusetts. Environ. Sci. Technol. 2017, 51 (8), 4269– 4279,  DOI: 10.1021/acs.est.6b05573
      35
      Geochemical and Hydrologic Factors Controlling Subsurface Transport of Poly- and Perfluoroalkyl Substances, Cape Cod, Massachusetts
      Weber, Andrea K.; Barber, Larry B.; LeBlanc, Denis R.; Sunderland, Elsie M.; Vecitis, Chad D.
      Environmental Science & Technology (2017), 51 (8), 4269-4279CODEN: ESTHAG; ISSN:0013-936X. (American Chemical Society)
      Growing evidence that certain poly- and perfluoroalkyl substances (PFASs) are assocd. with neg. human health effects prompted the U.S. Environmental Protection Agency to issue lifetime drinking water health advisories for perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS) in 2016. Given that groundwater is a major source of drinking water, the main objective of this work was to investigate geochem. and hydrol. processes governing the subsurface transport of PFASs at a former fire training area (FTA) on Cape Cod, Massachusetts, where PFAS-contg. aq. film-forming foams were used historically. A total of 148 groundwater samples and 4 sediment cores were collected along a 1200-m-long downgradient transect originating near the FTA, and analyzed for PFAS content. The results indicate that unsatd. zones at the FTA and at hydraulically downgradient former domestic wastewater effluent infiltration beds both act as continuous PFAS sources to the groundwater despite 18 and 20 years of inactivity, resp. Historically different PFAS sources are evident from contrasting PFAS compn. near the water table below the FTA and wastewater-infiltration beds. Results from total oxidizable precursor assays conducted using groundwater samples collected throughout the plume suggest that some perfluoroalkyl acid precursors at this site are transporting with perfluoroalkyl acids.
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    36. 36
      Shoari, N.; Dubé, J.-S. Toward Improved Analysis of Concentration Data: Embracing Nondetects. Environ. Toxicol. Chem. 2018, 37 (3), 643– 656,  DOI: 10.1002/etc.4046
      36
      Toward improved analysis of concentration data: Embracing nondetects
      Shoari, Niloofar; Dube, Jean-Sebastien
      Environmental Toxicology and Chemistry (2018), 37 (3), 643-656CODEN: ETOCDK; ISSN:0730-7268. (Wiley-Blackwell)
      Various statistical tests on concn. data serve to support decision-making regarding characterization and monitoring of contaminated media, assessing exposure to a chem., and quantifying the assocd. risks. However, the routine statistical protocols cannot be directly applied because of challenges arising from nondetects or left-censored observations, which are concn. measurements below the detection limit of measuring instruments. Despite the existence of techniques based on survival anal. that can adjust for nondetects, these are seldom taken into account properly. A comprehensive review of the literature showed that managing policies regarding anal. of censored data do not always agree and that guidance from regulatory agencies may be outdated. Therefore, researchers and practitioners commonly resort to the most convenient way of tackling the censored data problem by substituting nondetects with arbitrary consts. prior to data anal., although this is generally regarded as a bias-prone approach. Hoping to improve the interpretation of concn. data, the present article aims to familiarize researchers in different disciplines with the significance of left-censored observations and provides theor. and computational recommendations (under both frequentist and Bayesian frameworks) for adequate anal. of censored data. In particular, the present article synthesizes key findings from previous research with respect to 3 noteworthy aspects of inferential statistics: estn. of descriptive statistics, hypothesis testing, and regression anal. Environ Toxicol Chem 2018;9999:1-14. © 2017 SETAC.
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    37. 37
      Johnson, N.; Shelton, B. J.; Hopenhayn, C.; Tucker, T. T.; Unrine, J. M.; Huang, B.; Christian, W.; Zhang, Z.; Shi, X.; Li, L. Concentrations of Arsenic, Chromium, and Nickel in Toenail Samples from Appalachian Kentucky Residents. J. Environ. Pathol. Toxicol. Oncol. Off. organ Int. Soc. Environ. Toxicol. Cancer 2011, 30 (3), 213– 223,  DOI: 10.1615/JEnvironPatholToxicolOncol.v30.i3.40
      37
      Concentrations of arsenic, chromium, and nickel in toenail samples from Appalachian Kentucky residents
      Johnson Nancy; Shelton Brent J; Hopenhayn Claudia; Tucker Thomas T; Unrine Jason M; Huang Bin; Christian W; Zhang Zhuo; Shi Xianglin; Li Li
      Journal of environmental pathology, toxicology and oncology : official organ of the International Society for Environmental Toxicology and Cancer (2011), 30 (3), 213-23 ISSN:.
      Lung cancer rates in Appalachian Kentucky are almost twice national rates; colorectal cancer rates are also elevated. Although smoking prevalence is high, it does not explain all excess risk. The area is characterized by poverty, low educational attainment, and unemployment. Coal production is a major industry. Pyrite contaminants of coal contain established human carcinogens, arsenic (As), chromium (Cr), and nickel (Ni). We compared biological exposure to As, Cr, and Ni for adults living in Appalachian Kentucky with residents of Jefferson, a non-Appalachian, urban county. We further compared lung and colon cancer rates, demographics, and smoking prevalence across the study areas. Toenail clipping analysis measured As, Cr, and Ni for residents of 23 rural Appalachian Kentucky counties and for Jefferson County. Reverse Kaplan-Meier statistical methodology addressed left-censored data. Appalachian residents were exposed to higher concentrations of As, Cr, and Ni than Jefferson County residents. Lung cancer incidence and mortality rates in Appalachia are higher than Jefferson County and elsewhere in the state, as are colorectal mortality rates. Environmental factors may contribute to the increased concentration of trace elements measured in residents of the Appalachian region. Routes of human exposure need to be determined.
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    38. 38
      Ogawa, Y.; Tokunaga, E.; Kobayashi, O.; Hirai, K.; Shibata, N. Current Contributions of Organofluorine Compounds to the Agrochemical Industry. iScience 2020, 23 (9), 101467,  DOI: 10.1016/j.isci.2020.101467
      38
      Current Contributions of Organofluorine Compounds to the Agrochemical Industry
      Ogawa, Yuta; Tokunaga, Etsuko; Kobayashi, Osamu; Hirai, Kenji; Shibata, Norio
      iScience (2020), 23 (9), 101467CODEN: ISCICE; ISSN:2589-0042. (Elsevier B.V.)
      A review. Currently, more than 1,200 agrochems. are listed and many of these are regularly used by farmers to generate the food supply to support the expanding global population. However, resistance to pesticides is an ever more frequently occurring phenomenon, and thus, a continuous supply of novel agrochems. with high efficiency, selectivity, and low toxicity is required. Moreover, the demand for a more sustainable society, by reducing the risk chems. pose to human health and by minimizing their environmental footprint, renders the development of novel agrochems. an ever more challenging undertaking. In the last two decades, fluoro-chems. have been assocd. with significant advances in the agrochem. development process. We herein analyze the contribution that organofluorine compds. make to the agrochem. industry. Our database covers 424 fluoro-agrochems. and is subdivided into several categories including chemotypes, mode of action, heterocycles, and chirality. This in-depth anal. reveals the unique relationship between fluorine and agrochems.
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    39. 39
      Sandford, G. Organofluorine Chemistry. Philos. Trans. R. Soc. LONDON Ser. A-MATHEMATICAL Phys. Eng. Sci. 2000, 358 (1766), 455– 471,  DOI: 10.1098/rsta.2000.0541
      There is no corresponding record for this reference.
    40. 40
      Hammel, E.; Webster, T. F.; Gurney, R.; Heiger-Bernays, W. Implications of PFAS Definitions Using Fluorinated Pharmaceuticals. iScience 2022, 25 (4), 104020,  DOI: 10.1016/j.isci.2022.104020
      40
      Implications of PFAS definitions using fluorinated pharmaceuticals
      Hammel, Emily; Webster, Thomas F.; Gurney, Rich; Heiger-Bernays, Wendy
      iScience (2022), 25 (4), 104020CODEN: ISCICE; ISSN:2589-0042. (Elsevier B.V.)
      There are 9,000+ per- and polyfluoroalkyl substances (PFAS) in existence, which makes studying and regulating PFAS individually, or even as small mixts., infeasible. Multiple PFAS definitions based on structure have been proposed, yet these definitions do not consider the implications for the full suite of organofluorine chems. For example, organofluorine pharmaceuticals, whose use may be essential and are found in human serum and wastewater, are not uniformly identified across all definitions. Using nine definitions prepd. by various stakeholders, we screened the 360 organofluorine pharmaceuticals approved and used globally between 1954 and 2021. Definitions ranged in their inclusion of organofluorine pharmaceuticals (1%-100%). The most inclusive definitions include several top prescribed pharmaceuticals, e.g., Prozac and Lipitor. This anal. provides a framework against which organizations can make decisions about how best to proceed when defining PFAS.
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    41. 41
      Eriksson, U.; Karrman, A. World-Wide Indoor Exposure to Polyfluoroalkyl Phosphate Esters (PAPs) and Other PFASs in Household Dust. Environ. Sci. Technol. 2015, 49 (24), 14503– 14511,  DOI: 10.1021/acs.est.5b00679
      41
      World-Wide Indoor Exposure to Polyfluoroalkyl Phosphate Esters (PAPs) and other PFASs in Household Dust
      Eriksson, Ulrika; Kaerrman, Anna
      Environmental Science & Technology (2015), 49 (24), 14503-14511CODEN: ESTHAG; ISSN:0013-936X. (American Chemical Society)
      Human exposure to perfluorooctanoic acid (PFOA) and other per- and poly-fluoroalkyl substances (PFAS) is ongoing, in some cases increasing, despite efforts made to reduce emissions. The role of precursor compds., e.g., polyfluorinated phosphate esters (PAP), has received increasing attention, but there are knowledge gaps regarding their occurrence and impact on human exposure. This work compared mono-, di-, and triPAP, perfluorinated alkyl acids (PFAA), satd., and unsatd. fluorotelomer carboxylic acids (FTCA/FTUCA), perfluoroalkane sulfonamides, sulfonamidethanols (FOSA/FOSE), and 1 fluorotelomer sulfonic acid (FTSA) in household dust from Canada, the Faroe Islands, Sweden, Greece, Spain, Nepal, Japan, and Australia. Mono-, di-, and triPAP, including several diPAP homologues, were frequently detected in dust from all countries, revealing an ubiquitous spread in private households from diverse geog. areas, with significant differences among countries. Median monoPAP and diPAP concns. were 3.7-1023 ng/g and 3.6-692 ng/g, resp.; lowest concns. were obsd. in Nepal and highest in Japan. PAP concns. exceeded those of the other PFAS classes. Results showed the importance of PAP as a PFAS exposure source worldwide.
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    42. 42
      Hall, S. M.; Patton, S.; Petreas, M.; Zhang, S.; Phillips, A. L.; Hoffman, K.; Stapleton, H. M. Per- and Polyfluoroalkyl Substances in Dust Collected from Residential Homes and Fire Stations in North America. Environ. Sci. Technol. 2020, 54 (22), 14558– 14567,  DOI: 10.1021/acs.est.0c04869
      42
      Per- and polyfluoroalkyl substances in dust collected from residential homes and fire stations in North America
      Hall, Samantha M.; Patton, Sharyle; Petreas, Myrto; Zhang, Sharon; Phillips, Allison L.; Hoffman, Kate; Stapleton, Heather M.
      Environmental Science & Technology (2020), 54 (22), 14558-14567CODEN: ESTHAG; ISSN:0013-936X. (American Chemical Society)
      Over the past few years, human exposure to per- and polyfluoroalkyl substances (PFAS) has garnered increased attention. Research has focused on PFAS exposure via drinking water and diet, and fewer studies have focused on exposure in the indoor environment. To support more research on the latter exposure pathway, we conducted a study to evaluate PFAS in indoor dust. Dust samples from 184 homes in North Carolina and 49 fire stations across the United States and Canada were collected and analyzed for a suite of PFAS using liq. and gas chromatog.-mass spectrometry. Fluorotelomer alcs. (FTOHs) and di-polyfluoroalkyl phosphoric acid esters (diPAPs) were the most prevalent PFAS in both fire station and house dust samples, with medians of approx. 100 ng/g dust or greater. Notably, perfluorooctanesulfonic acid (PFOS), perfluorooctanoic acid (PFOA), perfluorohexane sulfonate, perfluorononanoic acid, and 6:2 diPAP were significantly higher in dust from fire stations than from homes, and 8:2 FTOH was significantly higher in homes than in fire stations. Addnl., when comparing our results to earlier published values, we see that perfluoroalkyl acid levels in residential dust appear to decrease over time, particularly for PFOA and PFOS. These results highlight a need to better understand what factors contribute to PFAS levels in dust and to understand how much dust contributes to overall human PFAS exposure.
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    43. 43
      Fraser, A. J.; Webster, T. F.; Watkins, D. J.; Strynar, M. J.; Kato, K.; Calafat, A. M.; Vieira, V. M.; McClean, M. D. Polyfluorinated Compounds in Dust from Homes, Offices, and Vehicles as Predictors of Concentrations in Office Workers’ Serum. Environ. Int. 2013, 60, 128– 136,  DOI: 10.1016/j.envint.2013.08.012
      43
      Polyfluorinated compounds in dust from homes, offices, and vehicles as predictors of concentrations in office workers' serum
      Fraser, Alicia J.; Webster, Thomas F.; Watkins, Deborah J.; Strynar, Mark J.; Kato, Kayoko; Calafat, Antonia M.; Vieira, Veronica M.; McClean, Michael D.
      Environment International (2013), 60 (), 128-136CODEN: ENVIDV; ISSN:0160-4120. (Elsevier Ltd.)
      We aimed to characterize levels of polyfluorinated compds. (PFCs) in indoor dust from offices, homes, and vehicles; to investigate factors that may affect PFC levels in dust; and to examine the assocns. between PFCs in dust and office workers' serum. Dust samples were collected in 2009 from offices, homes, and vehicles of 31 individuals in Boston, MA and analyzed for nineteen PFCs, including perfluorooctanoate (PFOA), perfluorooctane sulfonate (PFOS), fluorotelomer alcs. (FTOHs), and sulfonamidoethanols (FOSEs). Serum was collected from each participant and analyzed for eight PFCs including PFOA and PFOS. Perfluorononanoate, PFOA, perfluoroheptanoate, perfluorohexanoate, PFOS and 8:2 FTOH had detection frequencies > 50% in dust from all three microenvironments. The highest geometric mean concn. in office dust was for 8:2 FTOH (309 ng/g), while PFOS was highest in homes (26.9 ng/g) and vehicles (15.8 ng/g). Overall, offices had the highest PFC concns., particularly for longer-chain carboxylic acids and FTOHs. Perfluorobutyrate was prevalent in homes and vehicles, but not offices. PFOA serum concns. were not assocd. with PFC dust levels after adjusting for PFC concns. in office air. Dust concns. of most PFCs are higher in offices than in homes and vehicles. However, indoor dust may not be a significant source of exposure to PFCs for office workers. This finding suggests that our previously published observation of an assocn. between FTOH concns. in office air and PFOA concns. in office workers was not due to confounding by PFCs in dust.
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    44. 44
      Bohlin-Nizzetto, P.; Hanssen, L.; Herzke, D. PFASs in House Dust; NILU – Norwegian Institute for Air Research, 2015.
      There is no corresponding record for this reference.
    45. 45
      Jha, S. K.; Mishra, V. K.; Sharma, D. K.; Damodaran, T.; Whitacre, D. M. Fluoride in the Environment and Its Metabolism in Humans. Reviews of Environmental Contamination and Toxicology 2011, 211, 121– 142,  DOI: 10.1007/978-1-4419-8011-3_4
      45
      Fluoride in the environment and its metabolism in humans
      Jha, Sunil Kumar; Mishra, Vinay Kumar; Sharma, Dinesh Kumar; Damodaran, Thukkaram
      Reviews of Environmental Contamination and Toxicology (2011), 211 (), 121-142CODEN: RCTOE4; ISSN:0179-5953. (Springer)
      A review on the key factors that are responsible for fluoride exposure, including the problems caused by such exposure, and a description of how fluoride is absorbed and metabolized in humans.
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    46. 46
      Koch, A.; Aro, R.; Wang, T.; Yeung, L. W. Y. Towards a Comprehensive Analytical Workflow for the Chemical Characterisation of Organofluorine in Consumer Products and Environmental Samples. TrAC Trends Anal. Chem. 2020, 123, 115423,  DOI: 10.1016/j.trac.2019.02.024
      46
      Towards a comprehensive analytical workflow for the chemical characterisation of organofluorine in consumer products and environmental samples
      Koch, Alina; Aro, Rudolf; Wang, Thanh; Yeung, Leo W. Y.
      TrAC, Trends in Analytical Chemistry (2020), 123 (), 115423CODEN: TTAEDJ; ISSN:0165-9936. (Elsevier B.V.)
      A review. This review summarizes and discusses eight anal. methods for organofluorine (OF) anal., which offer detection limits suitable for consumer products and environmental samples. Direct sample anal. of OF only applies to some techniques on consumer products, whereas others require sample pre-treatment or concn. before measurements. Comparison between methods for OF anal. were found to be difficult because of different selectivity (between OF and fluoride), sensitivity and type of samples (bulk, ext., surface) analyzed. Neither inter-lab. comparison on OF anal. nor suitable certified ref. materials have been used for method validation, which makes data comparability between studies challenging. A top down approach for the comprehensive assessment of OF is proposed, where OF/extractable OF is first measured, followed by target anal. to obtain unquantifiable OF concns. using the mass balance approach. For further identification of unquantifiable OF, approaches such as total oxidizable precursor assay, suspect and non-target screening are briefly discussed.
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  • Supporting Information

    Supporting Information

    The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acs.est.2c05198.

    • Detailed description and tables of methods for analysis of 37 measured PFAS following the EOF extraction protocol (PDF)


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