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Download Hi-Res ImageDownload to MS-PowerPointCite This:J. Agric. Food Chem. 2015, 63, 18, 4449-4456
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Quantitative Screening of Agrochemical Residues in Fruits and Vegetables by Buffered Ethyl Acetate Extraction and LC-MS/MS Analysis

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National Referral Laboratory, ICAR−National Research Centre for Grapes, P.O. Manjri Farm, Pune 412307, India
*(K.B.) Phone: +91 20 2695 6091. Fax: +91 20 2695 6099. E-mail: [email protected].
Cite this: J. Agric. Food Chem. 2015, 63, 18, 4449-4456
Publication Date (Web):February 2, 2015
https://doi.org/10.1021/jf505221e
Copyright © 2015 American Chemical Society
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Abstract

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A buffered ethyl acetate extraction method is proposed for the simultaneous analysis of 296 agrochemicals in a wide range of fruit and vegetable matrices by liquid chromatography–tandem mass spectrometry (LC-MS/MS). The optimized quantity of acetate buffer (1% acetic acid + 0.5 g of sodium acetate per 10 g of sample) adjusted the pH of each test matrix to 5–6, which in turn significantly improved recoveries of acidic and basic compounds. The role of diethylene glycol (used in the evaporation step) on signal suppression of certain compounds was evaluated, and its quantity was optimized to minimize such an effect. The method was validated in grape, mango, drumstick, bitter gourd, capsicum, curry leaf, and okra as per the DG-SANCO/12571/2013 guidelines. Recoveries in the fortification range of 1–40 μg/kg were within 70–120% with associated relative standard deviations below 20% for most of the compounds. The method has potential for regulatory and commercial applications with a generic approach.

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Supplementary Figure S1: LC-MS/MS chromatogram of 296 agrochemicals in solvent standard at 10 ng/mL. Supplementary Figure S2: pH adjustment of matrices with diverse pH using optimized quantity of buffer. Supplementary Figure S3: effect on analyte response with respect to addition of variable volumes of diethylene glycol (DEG) solution (10%) during evaporation. Supplementary Figure S4: full scan analysis of standard methamidophos and DEG indicating coelution of DEG. Supplementary Figure S5: comparison of buffered QuEChERS and buffered ethyl acetate extraction methodologies. Supplementary Figure S6: comparative method performance for acidic and basic compounds in nonbuffered and buffered ethyl acetate extraction (I, recovery in grape, nonbuffered; II, recovery in grape, buffered; III, recovery in bitter gourd, nonbuffered; IV, recovery in bitter gourd, buffered; A, bispyribac; B, pymetrozine; C, cyromazine; D, atrazine desethyl 2-hydroxy). Supplementary Table S1: LC-MS/MS parameters of the test compoundsand. Supplementary Table S2. This material is available free of charge via the Internet at http://pubs.acs.org.

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