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Download Hi-Res ImageDownload to MS-PowerPointCite This:Anal. Chem. 2024, 96, 47, 18834-18841
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    Polarity Gradient Solvent Confinement Membrane Cartridge to Broaden Metabolite Coverage of Plasma Untargeted Analysis
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    • Chunyu Yu
      Chunyu Yu
      Department of Pharmaceutical Analysis, College of Pharmacy, Yanbian University, Yanji 133002, Jilin, China
      More by Chunyu Yu
    • Jiaxin Zhang
      Jiaxin Zhang
      Department of Pharmaceutical Analysis, College of Pharmacy, Yanbian University, Yanji 133002, Jilin, China
      More by Jiaxin Zhang
    • Xiaohan Zong
      Xiaohan Zong
      Department of Chemistry, Yanbian University, Yanji 133002, Jilin, China
      More by Xiaohan Zong
    • Xiangzi Jin
      Xiangzi Jin
      Department of Chemistry, Yanbian University, Yanji 133002, Jilin, China
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    • Lu Liu
      Lu Liu
      Department of Chemistry, Yanbian University, Yanji 133002, Jilin, China
      More by Lu Liu
    • Yilin Zou
      Yilin Zou
      Department of Chemistry, Yanbian University, Yanji 133002, Jilin, China
      More by Yilin Zou
    • Yifan Jiao
      Yifan Jiao
      Department of Chemistry, Yanbian University, Yanji 133002, Jilin, China
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    • Meihui Tong
      Meihui Tong
      Department of Chemistry, Yanbian University, Yanji 133002, Jilin, China
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    • Meiyu Cui
      Meiyu Cui
      Department of Chemistry, Yanbian University, Yanji 133002, Jilin, China
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    • Huwei Liu
      Huwei Liu
      College of Life Sciences, Wuchang University of Technology, Wuhan 430223, Hubei, China
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      Orcidhttps://orcid.org/0000-0001-6540-9657
    • Donghao Li*
      Donghao Li
      Department of Pharmaceutical Analysis, College of Pharmacy, Yanbian University, Yanji 133002, Jilin, China
      Department of Chemistry, Yanbian University, Yanji 133002, Jilin, China
      *Email: [email protected]. Tel: +86-433-2436456. Fax: +86-433-2432456.
      More by Donghao Li
      Orcidhttps://orcid.org/0000-0002-7033-6672
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    Analytical Chemistry

    Cite this: Anal. Chem. 2024, 96, 47, 18834–18841
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    https://doi.org/10.1021/acs.analchem.4c04400
    Published November 12, 2024
    Copyright © 2024 American Chemical Society
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    Abstract

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    Various polarity chemicals exist in complex samples, such as plasma; nontargeted comprehensive analysis naturally requires multiple polar-extracted solvents; consequently, the polarity of the solvent plays a crucial role in the extraction efficiency of analytes from complex samples. In the present study, based on the diffusion behavior and nanoconfinement effect of solvents in the nanoconfined space, the polarity gradient solvent confinement liquid-phase nanoextraction (PGSC-NLPNE) protocol aimed to perform a one-step nontargeted analysis of a wide range of metabolites in plasma was established. The continuously wide range of extracted solvent polarities on carbon nanofibers/carbon fiber (CNFs/CF) membranes was achieved using a mixture of hexane, dichloromethane, methanol, and water as nanoconfined solvents. The polarities (Log P) of gradient solvents ranged from −1.38 to 3.94. Correlational analyses indicated that metabolites with Log P values ranging from −1.90 to 3.84 were closely related according to similarity-intermiscibility theory. Coupled with a homemade modified guard column device, CNFs/CF membrane cartridge (CCMC), a PGSC-NLPNE-UHPLC-MS online protocol was established and applied in plasma untargeted analysis. By comparing metabolome coverage, reproducibility, and extraction recovery with protein precipitation and two-step liquid–liquid extraction commonly used in untargeted analysis, the PGSC-NLPNE-CCMC protocol demonstrated higher reproducibility and recovery. This protocol has shown great potential for ultrafast analysis of plasma untargeted metabolomics with broader metabolome coverage. It could be a potential tool to rapidly screen out valuable biomarkers related to diseases in the clinic.

    Copyright © 2024 American Chemical Society

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    Supporting Information

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    The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acs.analchem.4c04400.

    • Workflows of five plasma preparation methods; information of 68 metabolite standards (Table S1); the conditions of chromatography of UHPLC-QTOF-MS analysis (Table S2); the conditions of chromatography of HPLC-QQQ-MS analysis (Table S3); Log P values of pure and mixed solvents (Table S4); the CV values of 68 SQC standards (Table S5); the CV for peak intensities of SQC standards (Table S6); the differential metabolites extracted by the PGSC-NLPNE-CCMC protocol i (Table S7); the recovery (%) evaluation for SQC standards (Table S8); the comparison of the PGSC-NLPNE-CCMC protocol with classical methods (Table S9); SEM images of CNFs/CFs before the first extraction and after 10 recycles (Figure S1); the workflow of the PP method and two-step LLE method (Figure S2); the process of method evaluation (Figure S3); PLS-DA score plots of PGSC-NLPNE and two-step LLE method (Figure S4); and the recovery (%) evaluation for SQC standards (Figure S5) (PDF)

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    Analytical Chemistry

    Cite this: Anal. Chem. 2024, 96, 47, 18834–18841
    Click to copy citationCitation copied!
    https://doi.org/10.1021/acs.analchem.4c04400
    Published November 12, 2024
    Copyright © 2024 American Chemical Society
    Request reuse permissions

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