色谱

色谱 ›› 2017, Vol. 35 ›› Issue (10): 1086-1093.DOI: 10.3724/SP.J.1123.2017.06006

• 研究论文 • 上一篇    下一篇

改进的QuEChERS结合气相色谱-三重四极杆质谱法快速测定酸肉中10种挥发性N-亚硝胺类化合物

赵庄, 许杨彪, 刘向红, 施晓光, 鲁毅翔   

  1. 广西食品药品检验所, 广西 南宁 530021
  • 收稿日期:2017-06-01 出版日期:2017-10-08 发布日期:2017-10-18
  • 通讯作者: 鲁毅翔,E-mail:186424006@qq.com.
  • 基金资助:

    广西科技基础条件平台建设项目计划（12-112-01D）.

Rapid determination of 10 volatile N-nitrosamines in sour meats by modified QuEChERS and gas chromatography- triple quadrupole mass spectrometry

ZHAO Zhuang, XU Yangbiao, LIU Xianghong, SHI Xiaoguang, LU Yixiang   

  1. Guangxi Institute for Food and Drug Control, Nanning 530021, China
  • Received:2017-06-01 Online:2017-10-08 Published:2017-10-18
  • Supported by:

    Science and Technology Infrastructure and Facility Development Program of Guangxi (No. 12-112-01D).

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摘要：

采用改进的QuEChERS方法进行提取和净化，建立了气相色谱-三重四极杆质谱（GC-MS/MS）快速测定酸肉样品中10种挥发性N-亚硝胺类化合物的检测方法。样品经乙腈提取和正己烷除脂后，采用十八烷基硅烷键合硅胶（C18）和N-丙基乙二胺（PSA）混合吸附剂净化，采用DB-WAX色谱柱（30 m×0.25 mm×0.25 μm）分离，在选择反应监测（SRM）模式下进行测定，外标法定量。10种N-亚硝胺类化合物在1~100 μg/L范围内线性关系良好，相关系数（r）均＞0.99。10种N-亚硝胺类化合物的加标回收率为79.8%~115.3%，相对标准偏差（RSD）为0.6%~22.9%（n=6）；方法的检出限（LOD， S/N=3）和定量限（LOQ， S/N=10）分别为0.04~0.3 μg/kg和0.1~1 μg/kg。该法简便快速，灵敏有效，适用于酸肉中N-亚硝胺类化合物的快速筛查和测定。

关键词: N-亚硝胺类化合物, QuEChERS, 气相色谱-三重四极杆质谱, 酸肉

Abstract:

A rapid gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) method with modified QuEChERS method was developed for the determination of 10 volatile N-nitrosamines in sour meats. The samples were extracted with acetonitrile and eliminated the fat with n-hexane. The extracts in acetonitrile layer were purified by octadecyl silane (C18) and primary secondary amine (PSA) sorbents. The N-nitrosamines were determined on a DB-WAX column (30 m×0.25 mm×0.25 μm) by GC-MS/MS in selected reaction monitoring (SRM) mode. The external standard method was used to quantify the N-nitrosamines. The correlation coefficients (r) of the standard calibration curves were greater than 0.99 in the range of 1-100 μg/L. The average recoveries ranged from 79.8% to 115.3% with the relative standard deviations (RSDs) from 0.6% to 22.9% (n=6). The limits of detection (LODs, S/N=3) and limits of quantification (LOQs, S/N=10) were 0.04-0.3 μg/kg and 0.1-1 μg/kg, respectively. The developed method is simple, rapid, sensitive and efficient for the screening of the N-nitrosamines in sour meats.

Key words: N-nitrosamines, gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS), QuEChERS, sour meats

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