固相萃取-液相色谱-串联质谱法测定食品包装材料中16种全氟烷基类化合物  

Determination of 16 perfluorinated alkyl substances in food packaging materials by solid phase extraction-liquid chromatography-tandem mass spectrometry

作　　者：何建丽[1,2] 彭涛[1] 谢洁[1,3] 胡雪艳[1] 常巧英[1] 陈辉[1] 范春林[1] 李存[2] 

机构地区：[1]中国检验检疫科学研究院,北京100176 [2]天津农学院动物科学与动物医学学院,天津300384 [3]中国农业大学动物医学院,北京100193

出　　处：《色谱》2016年第7期708-714,共7页Chinese Journal of Chromatography

基　　金：国家科技基础性工作专项(2013FY113100)~~

摘　　要：建立了使用固相萃取-液相色谱-串联质谱(SPE-LC-MS/MS)同时检测食品包装材料中16种全氟烷基类化合物(PFAS)的方法。分别对样品前处理方法、质谱条件等进行了比较和优化,样品用甲醇超声提取,经Oasis WAX固相萃取小柱净化后,用Atlantis T3 C18色谱柱分离,以乙腈和5 mmol/L乙酸铵溶液为流动相进行梯度洗脱,多反应监测(MRM)负离子模式扫描,同位素内标法和外标法结合定量。16种PFAS在0.5~20.0μg/L范围内线性关系良好,相关系数(r^2)均大于0.99。加标回收率为68.6%~109.2%,RSD为2.5%~18.1%(n=6)。检出限为0.2~0.5μg/kg,定量限为0.5~1.0μg/kg。该方法简便、快速、准确,可用于食品包装材料样品中PFAS的检测。A method for the simultaneous determination of 16 perfluorinated alkyl substances（PFAS）in food packaging materials by solid phase extraction-liquid chromatography-tandem mass spectrometry（SPE-LC-MS / MS） was developed. Comparison and optimization of the sample pretreatment methods,mass spectrometry and other conditions were carried out. The samples were ultrasonically extracted with methanol,followed by clean-up using an Oasis WAX SPE column. The analytes were separated on a reversed phase Atlantis T3 C_（18） column and eluted gradiently with acetonitrile and 5 mmol / L ammonium acetate. The analytes were quantified using isotope internal standard and isotope external standard calibration curve method. The linear calibration curves were obtained in the range of 0. 5- 20. 0 μg / L with the linear relative coefficients more than 0.99. The recoveries were in the range of 68.6%-109.2% and the relative standard deviations（RSDs）were ranged from 2.5% to 18.1%（n = 6）. The limits of detection（LODs）and the limits of quantification（LOQs）for the PFAS were 0.2-0.5 μg/kg and 0.5-1.0μg / kg,respectively. This method is simple,rapid,accurate and can be used in the determination of PFAS in food packaging materials.

关 键 词：液相色谱-串联质谱 固相萃取 全氟烷基类化合物 包装材料 

分 类 号：O658[理学—分析化学]