[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]

Ying-Xiao Yue, Ya-Ting Bian, Yu-Fan Cheng, Lu He, Dan Wang, Pei-Xia Yan, Wei Yan, Gui-Ying Liu, Huan Song, Liang-Po Liu
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引用次数: 0

摘要

全氟和多氟烷基化合物(PFASs)是一类以其环境持久性而闻名的合成化学品。由于其疏水、疏油和耐高温的特性,全氟辛烷磺酸广泛应用于工业、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。全氟辛烷磺酸可在人体内积累,表现出多器官毒性。对毒性特征不明确的全氟辛烷磺酸的持续监测对于评估人类接触和相关健康风险至关重要。因此,建立一种高通量、高灵敏度的检测方法对于准确评估PFASs在人体内的暴露水平至关重要。本研究采用商用高通量hmr -脂质96孔固相萃取板,结合高效液相色谱-串联质谱(HPLC-MS/MS),建立了一种简便、高效的同时定量检测人血清中26种PFASs的方法。采用hmr -脂质96孔固相萃取板提取血清样品。采用Phenomenex C18色谱柱(250 mm×4.6 mm, 5 μm)作为捕获柱,连接在液相色谱混合器和自动进样器之间,避免高本底污染。目的化合物采用Accucore C18色谱柱(100 mm×2.4 mm, 2.6 μm)分离,采用负离子扫描模式电喷雾电离和多反应监测(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(r)为0.995 ~ 0.999 9。检测限(lod)为0.01 ~ 0.15 ng/mL,定量限(loq)为0.02 ~ 0.47 ng/mL。在低、中、高3个加标水平下,26种PFASs的加标回收率为80.1% ~ 119.5%,相对标准偏差(rsd)为0.5% ~ 11.9%。该方法具有灵敏度高、准确度好、操作简单、提取速度快、试剂用量少、所需样品量小等优点。适用于大规模人群生物监测,为准确评估全氟辛烷在人体内的暴露及其潜在健康风险提供了科学的方法支持。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

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

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

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.

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