色谱

色谱 ›› 2016, Vol. 34 ›› Issue (10): 998-1004.DOI: 10.3724/SP.J.1123.2016.07012

• 研究论文 • 上一篇    下一篇

分散固相萃取-气相色谱-串联质谱法测定动物源性食品中9种N-亚硝胺类化合物

赵博, 邓美林, 杨小珊, 段云鹏, 吴晓琴, 屠大伟   

  1. 重庆市食品药品检验检测研究院, 重庆市药物过程与质量控制工程技术研究中心, 重庆 401121
  • 收稿日期:2016-07-10 出版日期:2016-10-08 发布日期:2013-04-03
  • 通讯作者: 邓美林
  • 基金资助:

    重庆市食品药品检验检测研究院资助项目（SNKY-2015-07）.

Determination of nine N-nitrosamines in animal derived foods by dispersive solid-phase extraction-gas chromatography-tandem mass spectrometry

ZHAO Bo, DENG Meilin, YANG Xiaoshan, DUAN Yunpeng, WU Xiaoqin, TU Dawei   

  1. Chongqing Institute for Food and Drug Control; Chongqing Engineering Research Center for Pharmaceutical Process and Quality Control, Chongqing 401121, China
  • Received:2016-07-10 Online:2016-10-08 Published:2013-04-03
  • Supported by:

    Support Program of Chongqing Institute for Food and Drug Control (No. SNKY-2015-07).

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摘要：

建立了分散固相萃取-同位素稀释-气相色谱-串联质谱同时测定动物源性食品中9种N-亚硝胺的方法。样品用乙腈提取，上清液经分散固相萃取（dSPE）净化后浓缩。选用DB-WAX极性毛细管色谱柱对待测物进行分离，经EI源电离后以多反应监测（MRM）模式采集数据并做定性筛查和定量分析。9种N-亚硝胺在相应的浓度范围内线性关系良好，相关系数均大于0.99，对4类典型的动物源性食品进行3个不同浓度的加标试验，平均回收率为62.5%~118%，RSD为2.11%~25.6%，检出限（LOD，S/N=3）为0.02~0.31 μg/kg。该方法成本低廉、灵敏可靠，适用于同时对动物源性食品中9种N-亚硝胺进行定性和定量测定。

关键词: N-亚硝胺, 动物源性食品, 分散固相萃取, 气相色谱-串联质谱, 同位素稀释

Abstract:

A method has been developed and validated for the determination of nine N-nitrosamines in animal derived food using dispersive solid-phase extraction (dSPE) coupled with isotope dilution-gas chromatography-tandem mass spectrometry (GC-MS/MS). The samples were extracted by acetonitrile. The extracts were purified using mixed adsorbent by dSPE and then concentrated. The analytes were separated on a DB-WAX polar capillary column, and ionized by EI source. The data were collected by multiple reaction monitoring (MRM) mode, followed by qualitative screening and quantitative analysis. The correlation coefficients of linear calibration curves were over 0.99 in the corresponding linear ranges. Four kinds of typical animal derived foods were spiked at three levels. The average recoveries of the nine N-nitrosamines ranged from 62.5% to 118% with RSDs of 2.11%-25.6%. The limits of detection (LODs, S/N=3) were 0.02-0.31 μg/kg. The method is of low cost, sensitive, reliable, and suitable for the determination of nine N-nitrosamines in animal derived foods.

Key words: N-nitrosamines, animal derived foods, dispersive solid-phase extraction (dSPE), gas chromatography-tandem mass spectrometry (GC-MS/MS), isotope dilution

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