摘要
基于增强型脂质去除分散固相萃取净化法(EMR-Lipid dSPE)和超高效液相色谱串联三重四极杆质谱法(UPLC-MS/MS),建立了一种同时快速测定鱼肉中10种全氟烷基化合物(全氟十四烷酸、全氟十二烷酸、全氟十一烷酸、全氟壬酸、全氟辛酸、全氟己基磺酸、全氟庚酸、全氟己酸、全氟戊酸、全氟丁酸)残留的分析方法.样品以3.0 mL水+7.0 mL含0.1%甲酸的乙腈溶液为提取溶剂,EMR-Lipid dSPE净化,以Waters ACQUITY UPLC BEH C18色谱柱(1.7µm,2.1 mm×100 mm)分离,以乙腈–5 mmol/L乙酸铵的水溶液进行梯度洗脱,采用负离子电喷雾电离源采集,多反应监测模式进行检测.结果表明,10种全氟烷基化合物在各自浓度范围内均具有良好的线性关系,确定系数(R2)为0.9938~0.9998,检出限(LOD)为0.14~3.48μg/kg,定量限(LOQ)为0.48~11.40μg/kg,3个加标浓度水平的回收率为82.0%~119.2%,相对标准偏差(RSD)为1.1%~9.8%.该方法操作简单、快速、准确、高效,适用于筛查鱼肉中全氟烷基化合物的残留.
Based on the enhanced matrix removal-lipid dispersive solid-phase extraction(EMR-Lipid dSPE)method and ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS),an analytical method has been developed for the simultaneous and rapid determination of 10 perfluoroalkyl substances residues in fish,including perfluorotetradecanoic acid(PFTeDA),perfluorododecanoic acid(PFDoA),perfluoroundecanoic acid(PFUdA),perfluorononanoic acid(PFNA),perfluorooctanoic acid(PFOA),perfluorohexanesulfonic acid(PFHxS),perfluoroheptanoic acid(PFHpA),perfluorohexanoic acid(PFHxA),perfluoropentanoic acid(PFPeA),perfluorobutanesulfonic acid(PFBA).The samples were extracted by 3.0 mL water+7.0 mL acetonitrile solution containing 0.1%formic acid,purified by EMR-Lipid dSPE,separated by a Waters ACQUITY UPLC BEH C18 column(1.7µm,2.1 mm×100 mm)with a gradient elution of acetonitrile-5 mmol/L ammonium acetate of aqueous solution,and detected by multi-reaction monitoring mode of electrospray negative ions.The results showed that 10 perfluoroalkyl substances had a good linear relationship in their respective linear ranges,and the correlation coefficients were 0.9938~0.9998.The limits of detection were 0.14~3.48μg/kg,the limits of quantification were 0.48~11.40μg/kg.The spiked recoveries at three concentration levels were 82.0%~119.2%,with relative standard deviations of 1.1%to 9.8%.The method is simple,rapid,accurate and efficient,and is suitable for screening the residues of perfluoroalkyl substances in fish.
作者
许晓辉
李坚
王小乔
王瑞
王新娣
赵波
杜锐浒
李运
张生萍
刘光瑞
XU Xiaohui;LI Jian;WANG Xiaoqiao;WANG Rui;WANG Xindi;ZHAO Bo;DU Ruihu;LI Yun;ZHANG Shengping;LIU Guangrui(Lanzhou Institute for Food and Drug Control,Lanzhou 730050,China;Key Laboratory of Pesticide andVeterinary Drug Monitoring,State Administration for Market Regulation,Lanzhou 730050,China;GansuEngineering Research Center for Monitoring Exogenous Harmful Residues in Traditional Chinese Medicines,Lanzhou 730050,China;Gansu Provincal Acadamic Institute for Medical Research,Lanzhou 730050,China)
出处
《分析测试技术与仪器》
2025年第5期293-302,共10页
Analysis and Testing Technology and Instruments
基金
甘肃省市场监督管理局科技计划项目(SSCJG-SP-B202404,SSCJG-SP-B202302)。
关键词
超高效液相色谱串联三重四极杆质谱法
增强型脂质去除分散固相萃取净化法
全氟烷基化合物
ultra-high performance liquid chromatography-tandem mass spectrometry
enhanced matrix removal-lipid dispersion solid phase extraction
perfluoroalkyl substances
