HMR除脂-超高效液相色谱-串联质谱联用法测定食品中13种全氟和多氟烷基化合物  

Determination of 13 Per-and Polyfluoroalkyl Substances in Food by HMR Degreasing-ultra Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：崔淑丹 赖淼菊 祝欣然 欧阳赵逸 万怡汶 李强[1] CUI Shudan;LAI Miaoju;ZHU Xinran;OUYANG Zhaoyi;WAN Yiwen;LI Qiang(Physical and Chemical Department,Shanghai Putuo District Center for Disease Control and Prevention,Shanghai 200333,China)

机构地区：[1]上海市普陀区疾病预防控制中心理化检验科,上海200333

出　　处：《广州化工》2025年第6期92-97,共6页GuangZhou Chemical Industry

基　　金：上海市普陀区卫生健康系统公共卫生青年课题(ptgw202305)。

摘　　要：建立适用肉类、水产、蔬菜、水果、谷物、奶类和蛋类样品中13种全氟和多氟烷基化合物的超高效液相色谱-串联质谱测定法。食品样品经乙腈提取,离心后上清液用HMR-Lipid固相萃取柱净化,过滤液用水稀释,过0.22μm再生纤维素滤膜。目标物经Waters ACQUITY Premier BEH C_(18)液相色谱柱分离后,在电喷雾离子源负离子模式下通过多反应监测方式检测,同位素内标法定量。13种PFAS在0.1~2.0μg/L的浓度范围内线性良好,相关系数r>0.995,检出限在0.01~0.20μg/kg之间,定量限在0.02~0.68μg/kg之间,13种PFAS的平均回收率在70.0%~130%之间,相对标准偏差在0.72%~9.97%之间。该方法前处理简单、灵敏度高、重现性好,适用于多种食品中PFAS污染的筛查与测定。An ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of 13 per-and polyfluoroalkyl substances(PFAS)in meat,aquatic products,vegetables,fruits,grains,dairy,and eggs were established.Food samples were extracted with acetonitrile,and the supernatant was purified using an HMRlipid solid-phase extraction column after centrifugation.The filtrate was diluted with water and passed through a 0.22μm regenerated cellulose membrane.Target analytes were separated on a Waters ACQUITY Premier BEH C_(18) column and detected in negative electrospray ionization mode using multiple reaction monitoring(MRM).Quantification was performed using isotope-labeled internal standards.13 PFAS showed good linearity in the concentration range of 0.1 to 2.0μg/L,with correlation coefficients(r)>0.995.The limits of detection(LODs)ranged from 0.01 to 0.20μg/kg,and the limits of quantification(LOQs)ranged from 0.02 to 0.68μg/kg.The average recoveries of 13 PFAS were between 70.0%and 130%,with relative standard deviations(RSDs)ranging from 0.72%to 9.97%.This method is simple,sensitive and reproducible,making it suitable for screening and determining PFAS contamination in various food samples.

关 键 词：食品 固相萃取 全氟和多氟烷基化合物 高效液相色谱-串联质谱 

分 类 号：O657.7[理学—分析化学]