分散固相萃取结合高效液相色谱-串联质谱法测定羊肝中19种全氟烷基酸

doi:10.3724/SP.J.1123.2014.12034

色谱 ›› 2015, Vol. 33 ›› Issue (5): 494-500.DOI: 10.3724/SP.J.1123.2014.12034

分散固相萃取结合高效液相色谱-串联质谱法测定羊肝中19种全氟烷基酸

朱萍萍^1,2, 岳振峰¹, 郑宗坤², 张毅¹, 黎文茵^1,2, 赵凤娟¹, 肖陈贵¹, 白润叶^1,2, 林蔚^1,2

1. 深圳出入境检验检疫局食品检验检疫技术中心, 深圳市食品安全检测技术研发重点实验室, 广东深圳 518045;
2. 深圳大学化学与化工学院, 广东深圳 518060

收稿日期:2014-12-25 修回日期:2015-03-18 出版日期:2015-05-08 发布日期:2015-04-23
通讯作者: 岳振峰
基金资助:
国家科技基础性工作专项重点项目(2013FY113100);科技部"十二五"科技支撑计划项目(2012BAD33B02).

Determination of perfluoroalkyl acids in lamb liver by high performance liquid chromatography-tandem mass spectrometry combined with dispersive solid phase extraction

ZHU Pingping^1,2, YUE Zhenfeng¹, ZHENG Zongkun², ZHANG Yi¹, LI Wenyin^1,2, ZHAO Fengjuan¹, XIAO Chengui¹, BAI Runye^1,2, LIN Wei^1,2

1. Food Inspection and Quarantine Center, Shenzhen Entry-Exit Inspection and Quarantine Bureau; Shenzhen Key Laboratory of Detection Technology R. & D. on Food Safety, Shenzhen 518045, China;
2. College of Chemistry and Chemical Engineering, Shenzhen University, Shenzhen 518060, China

Received:2014-12-25 Revised:2015-03-18 Online:2015-05-08 Published:2015-04-23

摘要/Abstract

摘要：

建立了羊肝样品中19种全氟烷基酸(PFAs)的高效液相色谱-串联质谱检测方法。样品经酸化乙腈提取,加入乙二胺-N-丙基硅烷(PSA)、C18、石墨化炭黑(GCB)3种吸附剂后涡旋振荡对样品进行净化。以高效液相色谱-串联质谱(HPLC-MS/MS)检测萃取液中PFAs含量,采用C18色谱柱分离,负离子模式电喷雾电离,配合多级反应离子扫描(MRM)定性分析目标化合物。考察了盐酸和吸附剂的用量对加标回收率的影响,优化了主要影响因素和实验条件。在优化条件下采用同位素标记内标物进行定量分析。19种PFAs在0.05~20 μg/kg范围内线性关系良好,相关系数R>0.998,检出限(LOD)为0.004~0.111 μg/kg,定量限(LOQ)为0.012~0.370 μg/kg。在0.5、1.0、2.0 μg/kg加标水平下,19种PFAs的加标回收率为80%~128%,相对标准偏差(RSD)范围为0.31%~11.1%。该方法快速、简单、准确,适用于羊肝样品中19种PFAs的检测分析。

关键词: 分散固相萃取, 高效液相色谱-串联质谱, 全氟烷基酸, 羊肝

Abstract:

A method was developed for the determination of 19 perfluoroalkyl acids (PFAs) in lamb liver by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) combined with dispersive solid phase extraction. The sample was extracted with acidified acetonitrile, and then cleaned-up by a mixture of N-propylethylenediamine (PSA), C18 and graphitized carbon black (GCB) sorbents. The 19 PFAs were analyzed by HPLC-MS/MS with a C18 chromatographic column, adopting the multiple reaction monitoring (MRM) mode with negative electrospray ionization. The effects of the dosages of hydrochloric acid and the sorbents on the recoveries of the 19 PFAs were studied. For accurate quantitative analysis, the isotope internal standard method was used. The calibration curves were linear with the correlation coefficients over 0.998 in the range of 0.05-20 μg/kg for the 19 PFAs. The limits of detection were 0.004-0.111 μg/kg. The limits of quantification were 0.012-0.370 μg/kg. The mean recoveries of the 19 PFAs at spiked levels of 0.5, 1.0, 2.0 μg/kg were in the range from 80% to 128% with the relative standard deviations of 0.31%-11.1%. The developed method is rapid, simple, accurate. It is suitable for the determination of the 19 PFAs in large quantities of lamb liver samples.

Key words: dispersive solid phase extraction, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), lamb liver, perfluoroalkyl acids

中图分类号:

O658

朱萍萍, 岳振峰, 郑宗坤, 张毅, 黎文茵, 赵凤娟, 肖陈贵, 白润叶, 林蔚. 分散固相萃取结合高效液相色谱-串联质谱法测定羊肝中19种全氟烷基酸[J]. 色谱, 2015, 33(5): 494-500.

ZHU Pingping, YUE Zhenfeng, ZHENG Zongkun, ZHANG Yi, LI Wenyin, ZHAO Fengjuan, XIAO Chengui, BAI Runye, LIN Wei. Determination of perfluoroalkyl acids in lamb liver by high performance liquid chromatography-tandem mass spectrometry combined with dispersive solid phase extraction[J]. Chinese Journal of Chromatography, 2015, 33(5): 494-500.

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分散固相萃取结合高效液相色谱-串联质谱法测定羊肝中19种全氟烷基酸

Determination of perfluoroalkyl acids in lamb liver by high performance liquid chromatography-tandem mass spectrometry combined with dispersive solid phase extraction

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