高通量固相萃取-超高效液相色谱-串联质谱法测定血清中17种全氟/多氟烷基化合物  

Determination of 17 perfluorinated/polyfluoroalkyl compounds in serum by high-throughput solid-phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry

作　　者：林强 王健 李晶晶 苏东霞 李美丽 王佳 牛宇敏[3,4] 邵兵[3,4] LIN Qiang;WANG Jian;LI Jingjing;SU Dongxia;LI Meili;WANG Jia;NIU Yumin;SHAO Bing(Beijing Yanqing District Center for Disease Prevention and Control,Beijing 102100,China;Yongning Community Health Service Center in Beijing Yanqing District,Beijing 102100,China;Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning,Beijing Center for Disease Prevention and Control,Beijing 100013,China;School of Public Health,Capital Medical University,Beijing 100069,China)

机构地区：[1]北京市延庆区疾病预防控制中心,北京102100 [2]北京市延庆区永宁社区卫生服务中心,北京102100 [3]北京市疾病预防控制中心,食物中毒诊断溯源技术北京市重点实验室,北京100013 [4]首都医科大学公共卫生学院,北京100069

出　　处：《色谱》2025年第3期252-260,共9页Chinese Journal of Chromatography

基　　金：北京市科技计划课题(Z221100007122002);首都卫生发展科研专项(首发2022-2G-3016).

摘　　要：全氟烷基和多氟烷基化合物(PFASs)因其持久性、毒性和容易富集等特点,成为国内外广泛关注的一类新污染物。开展人体内PFASs的生物监测和暴露评估对于评估这些化学物质对人体健康的风险具有重要意义。因此亟需开发准确灵敏、方便快捷的检测方法。本研究采用自制的不需要活化、平衡的直通式HMR固相萃取柱净化样本,结合超高效液相色谱-串联质谱(UHPLC-MS/MS),建立了血清中17种PFASs的检测方法。50μL血清样本在HMR固相萃取柱中用400μL乙腈提取(每次200μL)并净化2次后,使用Poroshell 120 EC-C18色谱柱(100 mm×3 mm,2.7μm)分离,以5 mmol/L乙酸铵水溶液和甲醇为流动相进行梯度洗脱,ESI-离子源电离,采用多反应监测模式检测,同位素内标法定量。结果表明,17种PFASs在相应质量浓度范围内线性关系良好(r^(2)>0.995),检出限为3.6~14 ng/L,定量限为11~42 ng/L。血清样本加标回收率为89.3%~110.2%,日内相对标准偏差(RSD)为2.5%~9.8%,日间RSD为3.6%~10.2%。将方法应用于20份人体血清样品的检测,结果显示17种化合物均有检出。本方法仅需50μL血清样品,可以在HMR固相萃取柱中一步实现提取和净化,且固相萃取过程可以实现与96孔板的适配。方法操作简便,灵敏度高,样本用量少,检测效率高,适用于人群血清样本中PFASs的大规模监测及暴露评估。Perfluorinated/polyfluoroalkyl compounds(PFASs)are a group of synthetic chemicals.Since the 1940s,PFASs have been widely used in industrial and daily consumer fields.PFASs can enter the human body through various pathways,such as drinking water,food,and[HJ52x]air.Toxicological studies have shown that PFASs feature developmental and reproductive toxicity.Thus,the accurate assessment of PFAS exposure levels plays an important role in determining the health risks of these compounds.Biological monitoring is considered the most ideal means of monitoring and evaluating PFAS levels in the human body.The concentration of PFASs in serum can directly reflect their level of absorption in the human body after exposure;therefore,serum is widely used as a biological matrix for evaluating PFASs.In this study,a high-throughput solid-phase extraction(SPE)-ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)was developed for the determination of 17 PFASs in serum.A laboratory-made straight-through SPE column was used to purify serum samples.The SPE column used a new inorganic material with a low perfluorinated compound background.Unlike traditional SPE columns,the extraction column does not require activation before use,and the sample can be directly loaded into it for purification.The straight-through SPE column adopts a stepped design,which does not require a large sample volume and is suitable for the pretreatment of precious biological samples such as serum.The serum sample size adopted in this study was only 50μL,which is much lower than that required by other extraction methods.The straight-through SPE column can be used in conjunction with a 96-well plate,and the purification treatment of 96 serum samples can be completed within 30 min with high efficiency.LIN Qiang,WANG Jian,LI Jingjing,SU Dongxia,LI Meili,WANG Jia,NIU Yumin,SHAO Bing.Determination of 17 perfluorinated/polyfluoroalkyl compounds in serum by high-throughput solid-phase extraction-ultra-high performance liquid chromatography-tan

关 键 词：固相萃取 超高效液相色谱-串联质谱法 全氟/多氟烷基化合物 血清 

分 类 号：O658[理学—分析化学]