液-液萃取/气相色谱-串联质谱测定纸制食品接触材料中9种挥发性全氟化合物前体物的迁移量  

Analysis on Migration of 9 Volatile Perfluorinated Compounds Precursors in Food-contact Paper Based Materials by Gas Chromatography-Tandem Mass Spectrometry with Liquid-Liquid Extraction

作　　者：张子豪[1] 肖前[1] 钟怀宁[1] 李全忠[1] 刘莹峰[1] 李丹[1] 郑建国[1] ZHANG Zi-hao;XIAO Qian;ZHONG Huai-ning;LI Quan-zhong;LIU Ying-feng;LI Dan;ZHENG Jian-guo(Technical Centre of Guangdong Entry-Exit Inspection and Quarantine Bureau,Guangzhou 510623,China)

机构地区：[1]广东出入境检验检疫局,广东广州510623

出　　处：《分析测试学报》2018年第9期1002-1007,共6页Journal of Instrumental Analysis

基　　金：国家重点研发计划(2016YFF0203705)

摘　　要：采用气相色谱-串联质谱(GC-MS/MS)技术建立了纸制食品接触材料中全氟脂肪醇、全氟丙烯酸酯和全氟磺酰胺等9种挥发性全氟化合物前体物的测定方法。样品采用欧盟(EU) 2017/752中食品模拟物3%乙酸、10%乙醇、50%乙醇和橄榄油浸泡,水基模拟物用二氯甲烷萃取,橄榄油浸泡液用乙腈萃取,DB-5MS(30 m×0. 25 mm×0. 25μm)色谱柱分离后,采用多反应监测(MRM)模式进行检测。9种化合物在5~500μg/L质量浓度范围内与峰面积呈线性关系。在3%乙酸、10%乙醇、50%乙醇及橄榄油食品模拟物中的方法定量下限分别为3. 3~4. 4、3. 5~4. 2、3. 3~4. 9μg/L和4. 2~5. 1 ng/g。样品加标回收率为85. 0%~115%,相对标准偏差(RSD,n=6)≤7. 8%。该法快速可靠、准确简便,适用于纸制食品接触材料中全氟化合物前体物的分析检测。A gas chromatography-tandem mass spectrometric(GC-MS/MS)method was developed for the determination of 9 volatile perfluorinated compounds precursors including perfluorinated fatty alcohol,perfluorinated fatty alcohol acrylate and perfluorosulfonamide fatty alcohol,using 3%acetic acid,10%alcohol,50%alcohol,and olive oil as food simulants according to(EU)2017/752.The water-based and olive oil simulants were extracted with dichloromethane and acetonitrile,respectively.The volatile perfluorinated compounds precursors were separated on a DB-5MS(30 m×0.25 mm×0.25μm)column,and analyzed under multiple reaction monitoring mode.The cailbration curves for 9 analytes were linear in the range of 5-500μg/L,with the quantitation limits of 3.3-4.4μg/L for 3%acetic acid,3.5-4.2μg/L for 10%alcohol,3.3-4.9μg/L for 50%alcohol and 4.2-5.1 ng/g for olive oil,respectively.The spiked recoveries for the samples ranged from 85.0%to 115%with the relative standard deviations(RSDs)not more than 7.8%.This method was fast,precise and convenient,and was appropriate for the determination of 9 perfluorinated compounds precursors in food-contact paper based materials.

关 键 词：纸制食品接触材料 含氟化合物 前体物 迁移 液-液萃取 气相色谱-串联质谱(GC-MS/MS) 

分 类 号：O657.7[理学—分析化学] TS206.4[理学—化学]