磁性氧化石墨烯分散固相萃取/液相色谱-串联质谱法测定PVC儿童用品中内分泌干扰物迁移量  

Determination of Migration of Endocrine Disruptors in PVC Children Products by Liquid Chromatography-Tandem Mass Spectrometry with Magnetic Graphene Oxide Dispersive Solid Phase Extraction

作　　者：曹慧 张慧[2] 杨春 姜侃 王瑾 CAO Hui;ZHANG Hui;YANG Chun;JIANG Kan;WANG Jin(Zhejiang Institute of Product Quality and Safety Science,Hangzhou 310013,China;Zhejiang University of Science&Technology,Hangzhou 310023,China)

机构地区：[1]浙江省产品质量安全科学研究院,浙江杭州310013 [2]浙江科技学院,浙江杭州310023

出　　处：《分析测试学报》2022年第8期1207-1213,共7页Journal of Instrumental Analysis

基　　金：浙江省市场监督管理局NQI项目(20210101)。

摘　　要：建立了磁性氧化石墨烯分散固相萃取/液相色谱-串联质谱测定PVC儿童用品中14种内分泌干扰物迁移量的分析方法。样品经人工模拟汗液和人工模拟唾液浸泡,以磁性氧化石墨烯为分散固相萃取吸附剂,富集迁移液中的内分泌干扰物,采用液相色谱-串联质谱仪分析,基质外标法定量。结果表明:磁性氧化石墨烯用量10 mg,吸附15 min,采用3 mL含1%甲酸的丙酮洗脱15 min,可实现14种内分泌干扰物的富集与净化。14种内分泌干扰物在各自的质量浓度范围内线性关系良好,相关系数(r)为0.9901~0.9992,检出限为0.1~0.5μg/L,定量下限为0.3~1.5μg/L,加标回收率为80.2%~105%,相对标准偏差(RSD)为1.0%~6.8%。该方法操作简单、分析快速、重现性好,适用于PVC儿童用品中内分泌干扰物迁移量的测定。A method based on liquid chromatography-tandem mass spectrometry with magnetic graphene oxide dispersive solid phase extraction was developed for the determination of 14 kinds of endocrine disruptors in PVC children products.The samples were soaked in simulated sweat and simulated saliva,and the endocrine disruptors in migration fluid were enriched by magnetic graphene oxide dispersive solid phase extraction,determined by liquid chromatography-tandem mass spectrometry,and quantified by matrix external standard method.The results showed that 14 kinds of endocrine disruptors could be enriched and purified by a 15 min adsorption of 10 mg magnetic graphene oxide,and followed by a 15 min desorption of 3 mL acetone containing 1%formic acid.There were good linear relationships for the 14 analytes in the respective concentration ranges,with their correlation coefficients of 0.9901-0.9992.The limits of detection and limits of quantitation were in the range of 0.1-0.5μg/L and 0.3-1.5μg/L,respectively.Meanwhile,the spiked recoveries ranged from 80.2%to 105%,with relative standard deviations(RSDs)of 1.0%-6.8%.The method is simple,rapid and reproducible,and it could be used to determine the migration of endocrine disruptors in PVC children products.

关 键 词：液相色谱-串联质谱(LC-MS/MS) 磁性氧化石墨烯 内分泌干扰物 迁移量 PVC儿童用品 

分 类 号：O657.63[理学—分析化学] O657.7[理学—化学]