色谱

色谱 ›› 2025, Vol. 43 ›› Issue (9): 1005-1013.DOI: 10.3724/SP.J.1123.2024.10002

• 研究论文 • 上一篇    下一篇

固相萃取-高效液相色谱-串联质谱法测定人体血清中26种全氟及多氟烷基化合物

岳莹晓1, 边雅婷1, 成鱼帆1, 贺露1, 王丹1, 闫佩霞4, 闫伟1,2,3, 刘桂英1,2,3, 宋欢1,2,3, 刘良坡1,2,3,*()   

  1. 1.山西医科大学公共卫生学院卫生检验教研室，山西 太原 030001
    2.山西医科大学煤炭环境致病与防治教育部重点实验室，山西 太原 030001
    3.山西医科大学黄河流域生态公共卫生安全研究中心，山西 太原 030001
    4.北京市昌平区疾病预防控制中心，北京 102200
  • 收稿日期:2024-10-08 出版日期:2025-09-08 发布日期:2025-09-04
  • 通讯作者: *Tel：（0351）4135167，E-mail：lpliu@sxmu.edu.cn.
  • 基金资助:
    山西省应用基础研究计划项目(202203021221192);山西医科大学博士启动基金项目(XD1915)

Determination of 26 perfluorinated and polyfluoroalkyl compounds in human serum by solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry

YUE Yingxiao1, BIAN Yating1, CHENG Yufan1, HE Lu1, WANG Dan1, YAN Peixia4, YAN Wei1,2,3, LIU Guiying1,2,3, SONG Huan1,2,3, LIU Liangpo1,2,3,*()   

  1. 1. Department of Public Health Laboratory Sciences，School of Public Health，Shanxi Medical University，Taiyuan 030001，China
    2. Key Laboratory of Coal Environmental Pathogenicity and Prevention，Ministry of Education，Shanxi Medical University，Taiyuan 030001，China
    3. Center for Ecological Public Health Security of Yellow River Basin，Shanxi Medical University，Taiyuan 030001，China
    4. Beijing Changping District Center for Disease Prevention and Control，Beijing 102200，China
  • Received:2024-10-08 Online:2025-09-08 Published:2025-09-04
  • Supported by:
    Shanxi Province Applied Basic Research Program(202203021221192);Doctor Start-up Fund from Shanxi Medical University(XD1915)

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摘要：

全氟及多氟烷基化合物（PFASs）是一类由C-F键构成的人造化合物，具有高稳定性和难降解性，还具有生物累积性和多脏器毒性。因此，构建高通量、高灵敏度的检测方法，对于评估人体中PFASs的暴露水平至关重要。本研究采用商品化的高通量HMR-Lipid 96孔固相萃取板，结合高效液相色谱-串联质谱（HPLC-MS/MS），建立了一种简便、高效且能够同时定量检测人体血清中26种PFASs的方法。血清样本采用HMR-Lipid 96孔固相萃取板进行前处理，采用Phenomenex C18色谱柱（250 mm×4.6 mm， 5 μm）作为背景污染捕集柱，以Accucore C18色谱柱（100 mm×2.4 mm， 2.6 μm）作为分析柱，以2 mmol/L醋酸铵缓冲溶液和甲醇溶液作为流动相进行梯度洗脱。采用电喷雾电离、负离子扫描（ESI-）模式，在多反应监测（MRM）模式下进行定量分析。方法学验证结果表明，26种PFASs在0.2~100 ng/mL范围内线性关系良好，相关系数为0.995 1~0.999 9，检出限（LOD）和定量限（LOQ）分别为0.01~0.15 ng/mL和0.02~0.47 ng/mL。在低（5 ng/mL）、中（10 ng/mL）、高（50 ng/mL）3个加标水平下，26种PFASs的回收率为80.1%~119.5%，相对标准偏差（RSD）为0.5%~11.9%。与传统固相萃取方法相比，本研究建立的方法具有灵敏度高、准确性好、操作简便、萃取速度快、试剂消耗少以及所需样品量小等优点，适用于大规模人群生物监测，为准确评估人体中PFASs的暴露情况及其潜在健康风险提供了科学的方法支撑。

关键词: HMR-Lipid 96孔固相萃取板, 高效液相色谱-串联质谱法, 全氟及多氟烷基化合物, 人体血清

Abstract:

Perfluorinated and polyfluoroalkyl compounds （PFASs） represent a category of synthetic chemicals renowned for their environmental persistence. Owing to their hydrophobic， oleophobic， and high-temperature-resistant properties， PFASs are extensively utilized in industrial， agricultural， and civilian sectors， including applications in leather， textiles， flame-retardant materials， lubricants， and coatings， among others. PFASs can accumulate within the human body， exhibiting multi-organ toxicity. Continuous monitoring of PFASs with ambiguous toxicity profiles is vital for evaluating human exposure and associated health risks. Consequently， the establishment of a high-throughput and highly sensitive detection method is of paramount importance for accurately assessing the exposure levels of PFASs in the human body. In this study， a commercial high-throughput HMR-Lipid 96-well solid-phase extraction plate was adopted， combined with high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）， to establish a simple， efficient method that can simultaneously quantitatively detect 26 PFASs in human serum. Serum samples were extracted using the HMR-lipid 96-well solid-phase extraction plate. The Phenomenex C18 chromatography column （250 mm×4.6 mm， 5 μm） was used as the capture column and connected between the liquid chromatography mixer and the autosampler to avoid high background pollution. The target compounds were separated by the Accucore C18 chromatography column （100 mm×2.4 mm， 2.6 μm） and analyzed using the electrospray ionization with negative ion scanning mode and multiple reaction monitoring （MRM） mode. The methodological validation results indicated that the 26 PFASs had good linear relationships within the range of 0.2-100 ng/mL， with correlation coefficients （r） of 0.995 1-0.999 9. The limits of detection （LODs） and quantification （LOQs） were 0.01-0.15 ng/mL and 0.02-0.47 ng/mL， respectively. At three spiked levels of low， medium and high， the recoveries of the 26 PFASs ranged from 80.1% to 119.5%， and the relative standard deviations （RSDs） ranged from 0.5% to 11.9%. This method has the advantages of high sensitivity， good accuracy， simple operation， fast extraction speed， low reagent consumption and small sample volume required. It is suitable for large-scale population biological monitoring and provides a scientific method support for accurately assessing the exposure of PFASs in the human body and its potential health risks.

Key words: HMR-lipid 96-well solid-phase extraction plate, high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）, perfluorinated and polyfluoroalkyl compounds （PFASs）, human serum

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