色谱 ›› 2019, Vol. 37 ›› Issue (2): 207-215.DOI: 10.3724/SP.J.1123.2018.09037

• 研究论文 • 上一篇    下一篇

气相色谱-串联质谱法测定肉制品中10种挥发性N-亚硝胺类化合物

朱萌萌1, 叶群2, 周婷婷1, 陈卢涛1, 俞璐萍1, 黎斌1, 胡晋峰3, 周敏1   

  1. 1. 绿城农科检测技术有限公司, 浙江 杭州 310000;
    2. 浙江茗皇天然食品开发股份有限公司, 浙江 杭州 310000;
    3. 安徽农业大学茶与食品科技学院, 茶叶生物与利用国家重点实验室, 安徽 合肥 230036
  • 收稿日期:2018-09-29 出版日期:2019-02-09 发布日期:2014-12-31
  • 通讯作者: 周敏,E-mail:66871505@qq.com

Determination of 10 volatile N-nitrosamines in meat products by gas chromatography-tandem mass spectrometry

ZHU Mengmeng1, YE Qun2, ZHOU Tingting1, CHEN Lutao1, YU Luping1, LI Bin1, HU Jinfeng3, ZHOU Min1   

  1. 1. Greentown Agricultural Detection Technology Co., Ltd., Hangzhou 310000, China;
    2. Zhejiang Minghuang Natural Products Development Co., Ltd. Hangzhou 310000, China;
    3. State Key Laboratory of Tea Plant Biology and Utilization, College of Tea and Food Science & Technology, Anhui Agricultural University, Hefei 230036, China
  • Received:2018-09-29 Online:2019-02-09 Published:2014-12-31

摘要:

建立了气相色谱-串联质谱(GC-MS/MS)检测肉制品中10种挥发性N-亚硝胺类化合物残留量的方法。肉制品样品经同时蒸馏萃取法(SDE)萃取,采用冷冻去脂净化法,在多反应监测模式下分析,外标法定量。结果表明,采用优化后的条件,10种挥发性N-亚硝胺类化合物在1.00~1000 μg/L范围内线性关系良好,相关系数均在0.99以上。方法的检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.01~0.02 μg/kg和0.04~0.07 μg/kg。选取3种不同类型的肉制品(火腿肠、中式香肠和腌渍腊肉),在空白样品添加水平为LOQ水平、1.0、2.0 μg/kg时,10种挥发性N-亚硝胺类化合物的平均回收率为74.8%~94.3%,相对标准偏差小于8.3%。市售3类肉制品中6种挥发性N-亚硝胺类化合物(N-亚硝基二甲胺、N-亚硝基二乙胺、N-亚硝基吡咯烷、N-亚硝基哌啶、N-亚硝基二丁胺、N-亚硝基二丙胺)均有不同程度检出,且腌渍腊肉中每种挥发性N-亚硝胺类化合物的检出值最高。该方法操作简单,萃取充分,灵敏度高,试剂用量少,可满足实验室大量样品的日常检测需求。

关键词: N-亚硝胺类化合物, 冷冻去脂, 气相色谱-串联质谱, 肉制品, 同时蒸馏萃取

Abstract:

A gas chromatography-tandem mass spectrometry (GC-MS/MS) method was established for the determination of 10 volatile N-nitrosamines in meat products. The meat samples were extracted by simultaneous distillation extraction (SDE), and then a cleanup step involving the frozen fat removal method was applied. The analytes were quantified by the external standard method in multiple reaction monitoring (MRM) mode. Under the optimized conditions, the correlation coefficients of the standard calibration curves were greater than 0.99 in the range of 1.00-1000 μg/L. The limits of detection (LODs, S/N=3) and limits of quantification (LOQs, S/N=10) were 0.01-0.02 μg/kg and 0.04-0.07 μg/kg, respectively. The average spiked recoveries of the 10 volatile N-nitrosamines were 74.8%-94.3% at spiked levels of LOQ level, 1.0 and 2.0 μg/kg,and the relative standard deviations were less than 8.3%. Six volatile N-nitrosamines (N-nitrosodimethylamine (NDMA), N-nitrosodiethylamine (NDEA), N-nitrosopyrrolidine (NPYR), N-nitrosopiperidine (NPIP), N-nitrosodibutylamine (NDBA) and N-nitrosodi-n-propylamine (NDPA)) were detected in different types of meat products, and each volatile N-nitrosamine in pickled meat products had the highest detection values. The developed method has the advantages of simplicity, sufficient extraction, high sensitivity, and low reagent dosage, in addition to proving suitable for the daily testing requirements of a large number of samples in the laboratory.

Key words: N-nitrosamines, freezing lipid filtration, gas chromatography-tandem mass spectrometry (GC-MS/MS), meat products, simultaneous distillation extraction (SDE)

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