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[固相萃取-高效液相色谱-串联质谱法测定人血清中26种全氟和多氟烷基化合物]

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

作者信息

Yue Ying-Xiao, Bian Ya-Ting, Cheng Yu-Fan, He Lu, Wang Dan, Yan Pei-Xia, Yan Wei, Liu Gui-Ying, Song Huan, Liu Liang-Po

机构信息

Department of Public Health Laboratory Sciences,School of Public Health,Shanxi Medical University,Taiyuan 030001,China.

Beijing Changping District Center for Disease Prevention and Control,Beijing 102200,China.

出版信息

Se Pu. 2025 Sep;43(9):1005-1013. doi: 10.3724/SP.J.1123.2024.10002.

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 C 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 C 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 () 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.

摘要

全氟和多氟烷基化合物(PFASs)是一类以环境持久性著称的合成化学品。由于其疏水、疏油和耐高温特性,PFASs被广泛应用于工业、农业和民用领域,包括皮革、纺织品、阻燃材料、润滑剂和涂料等方面。PFASs可在人体内蓄积,表现出多器官毒性。持续监测毒性特征尚不明确的PFASs对于评估人体暴露情况及相关健康风险至关重要。因此,建立一种高通量且高灵敏度的检测方法对于准确评估人体中PFASs的暴露水平至关重要。在本研究中,采用商用高通量HMR-脂质96孔固相萃取板,结合高效液相色谱-串联质谱法(HPLC-MS/MS),建立了一种能同时定量检测人血清中26种PFASs的简单、高效方法。血清样品用HMR-脂质96孔固相萃取板进行萃取。使用Phenomenex C色谱柱(250 mm×4.6 mm,5μm)作为捕获柱,连接在液相色谱混合器和自动进样器之间,以避免高背景污染。目标化合物通过Accucore C色谱柱(100 mm×2.4 mm,2.6μm)进行分离,并采用电喷雾电离负离子扫描模式和多反应监测(MRM)模式进行分析。方法学验证结果表明,26种PFASs在0.2 - 100 ng/mL范围内具有良好的线性关系,相关系数()为0.995 1 - 0.999 9。检测限(LODs)和定量限(LOQs)分别为0.01 - 0.15 ng/mL和0.02 - 0.47 ng/mL。在低、中、高三个加标水平下,26种PFASs的回收率为80.1%至119.5%,相对标准偏差(RSDs)为0.5%至11.9%。该方法具有灵敏度高、准确性好、操作简单、萃取速度快、试剂消耗低和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的暴露及其潜在健康风险提供了科学的方法支持。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/0f0b/12412018/d7d3d024d837/3AAC8E83-011E-4191-996E-FB14FE554ED7-F001.jpg

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