Determination of 43 Persistent Organochlorine Pollutants in Human Serum by Gas Chromatography－Tandem Mass Spectrometry

QIU Tian; BAO Shan; JIANG Wei-long; LU Yi-fu

doi:10.19969/j.fxcsxb.23031003

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Determination of 43 Persistent Organochlorine Pollutants in Human Serum by Gas Chromatography－Tandem Mass Spectrometry

Scientific Papers | 更新时间：2023-07-12

- Determination of 43 Persistent Organochlorine Pollutants in Human Serum by Gas Chromatography－Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 42, Issue 7, Pages: 775-783(2023)
- 作者机构：
  
  1.中国疾病预防控制中心环境与人群健康重点实验室，中国疾病预防控制中心环境与健康相关产品安全所，北京 100021
  2.安徽医科大学公共卫生学院，安徽合肥 230032
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.23031003
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邱天,鲍珊,姜威龙等.气相色谱－串联质谱法测定人血清中43种持久性有机氯污染物[J].分析测试学报,2023,42(07):775-783.

QIU Tian,BAO Shan,JIANG Wei-long,et al.Determination of 43 Persistent Organochlorine Pollutants in Human Serum by Gas Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(07):775-783.
邱天,鲍珊,姜威龙等.气相色谱－串联质谱法测定人血清中43种持久性有机氯污染物[J].分析测试学报,2023,42(07):775-783. DOI： 10.19969/j.fxcsxb.23031003.

QIU Tian,BAO Shan,JIANG Wei-long,et al.Determination of 43 Persistent Organochlorine Pollutants in Human Serum by Gas Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(07):775-783. DOI： 10.19969/j.fxcsxb.23031003.

摘要

建立了基于液液萃取－固相萃取净化同时测定人血清中43种持久性有机氯污染物（POCPs）的气相色谱－串联质谱（GC－MS/MS）方法，包含18种多氯联苯（PCBs）和25种有机氯农药（OCPs）。取250 μL血清样本加入甲醇和酸，使用正己烷和甲基叔丁基醚依次对样品进行萃取，硅胶固相萃取柱对提取液进行净化，洗脱液氮吹浓缩后用甲苯复溶，经TG-5SilMS（30 m × 0.25 mm × 0.25 μm）毛细管色谱柱分离，多反应监测（MRM）模式下进行测定，内标法定量。结果表明，18种PCBs和25种OCPs分别在0.008 ~ 1 µg/L和0.08 ~ 10 µg/L范围内线性关系良好，方法检出限为0.005 ~ 0.1 µg/L，定量下限为0.02 ~ 0.3 µg/L，基质效应为74.9% ~ 126%；加标回收率为71.6% ~ 129%，日内相对标准偏差（RSD）为1.0% ~ 11%，日间RSD为1.3% ~ 18%。使用标准参考样品评估方法准确度，测定结果与参考值的相对偏差均小于30%。应用该方法测定某地区173份普通人群血清样品，共检出28种POCPs，其中,p,，,p,'-DDE和PCB153的检出率超过50%，,p，p',-DDE质量浓度的中位数为0.46 μg/L，是该地区人群血清中主要的POCPs组分。该方法可有效控制基质效应，提高检测灵敏度，适用于人血清中43种POCPs的检测。

Abstract

A gas chromatography－tandem mass spectrometric（GC－MS/MS） method was developed for the simultaneous analysis of 43 persistent organochlorine pollutants（POCPs），including 18 polychlorinated biphenyls（PCBs） and 25 organochlorine pesticides（OCPs） in human serum，based on solvent extraction coupled with solid-phase extraction cartridge cleanup．Human serum samples were thawed and brought to room temperature before pretreatment．An aliquot of 250 µL serum sample was transferred into a 12 mL glass tube．Protein was precipitated using methanol and lipid was removed by acidification to release target analytes．A liquid－liquid extraction was performed using hexane and methyl ,tert,-butyl ether in turn．The extract from both solvent was combined and concentrated．The sample was further purified using silica gel solid-phase extraction cartridges，then concentrated to near-dryness under gentle stream of nitrogen and reconstituted with toluene．Subsequently，the chromatographic separation was performed on a TG-5SilMS（30 m × 0.25 mm × 0.25 µm） column．The target analytes were monitored under multiple reaction monitoring（MRM） mode，and quantified by internal standard method．The results showed that there were good linear relations for the 18 PCBs and 25 OCPs in the ranges of 0.008－1 µg/L and 0.08－10 µg/L，with the detection limits and the quantitation limits of 0.005－0.1 µg/L and 0.02－0.3 µg/L，respectively．The matrix effect was in the range of 74.9%－126%．The spiked recoveries ranged from 71.6% to 129%，with intra-day relative standard deviations（RSDs） and inter-day RSDs of 1.0%－11% and 1.3%－18%，respectively．To evaluate method accuracy，standard reference material purchased from the US National Institute of Standards and Technology was used．The relative deviations of tested results were lower than 30% compared to certified values．The developed method was applied to the determination of 173 serum samples collected from general population．A total of 28 POCPs were detected，of which ,p,，,p,′-DDE and PCB 153 both had a detection frequency over 50%，and the median concentration of ,p,，,p,′-DDE was found to be 0.46 µg/L，making it the primary POCPs in the serum samples of this particular population．This analytical method is suitable for the detection on 43 POCPs in human serum samples as it could effectively control the matrix effect and improve the analytical sensitivity.

关键词

气相色谱－串联质谱持久性有机氯污染物液液萃取固相萃取人血清

Keywords

gas chromatography－tandem mass spectrometrypersistent organochlorine pollutantsliquid－liquid extractionsolid-phase extractionhuman serum

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