色谱

色谱 ›› 2013, Vol. 31 ›› Issue (3): 223-227.DOI: 10.3724/SP.J.1123.2012.10020

• 研究论文 • 上一篇    下一篇

气相色谱-质谱联用法测定腌制水产品中的挥发性N-亚硝胺类化合物

赵华1, 王秀元2*, 王萍亚1, 周勇1, 薛超波1, 蒋玲波1   

  1. 1. 国家海洋食品质量监督检验中心, 浙江 舟山 316021; 2. 浙江海洋学院食品与医药学院, 浙江 舟山 316000
  • 收稿日期:2012-10-25 修回日期:2012-11-19 出版日期:2013-03-28 发布日期:2013-03-22
  • 通讯作者: 赵华
  • 基金资助:

    科技部公益专项课题(201210060);浙江省质量技术监督系统科研计划项目(20110243).

Determination of volatile N-nitrosamine compounds in salted aquatic products by gas chromatography-mass spectrometry

ZHAO Hua1, WANG Xiuyuan2*, WANG Pingya1, ZHOU Yong1, XUE Chaobo1, JIANG Lingbo1   

  1. 1. National Marine Food Quality Supervision and Testing Center, Zhoushan 316021, China; 2. School of Food and Pharmacy & Medical School, Zhejiang Ocean University, Zhoushan 316000, China
  • Received:2012-10-25 Revised:2012-11-19 Online:2013-03-28 Published:2013-03-22
  • Contact: Hua ZHAO

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651

被引次数

44

摘要： 建立了气相色谱-质谱(GC-MS)快速测定腌制水产品中挥发性N-亚硝胺含量的分析方法。采用GC-MS测定了N-二甲基亚硝胺(NDMA)、N-二乙基亚硝胺(NDEA)、N-二丙基亚硝胺(NDPA)、N-亚硝基吡咯烷(NPYR)、N-亚硝基哌啶(NPIP)、N-二丁基亚硝胺(NDBA)6种化合物,考察了样品不同提取方法、不同固相萃取小柱、不同色谱柱对分离检测的影响。结果显示: 在10～1000 μg/L范围内,线性相关系数可达0.9998以上;重现性良好,相对标准偏差小于8%;回收率可达79%～105%;灵敏度高,检出限低,除NDPA为0.03 μg/kg外,其他5种N-亚硝胺为0.05 μg/kg。该方法前处理快速简捷,易于操作,适用于腌制水产品中N-亚硝胺残留量的检测工作。

关键词: N-亚硝胺, 气相色谱-质谱, 腌制水产品

Abstract: An analytical method was developed for the determination of the extraction of volatile N-nitrosamine compounds including N-nitrosodimethylamine (NDMA), N-nitrosodiethylamine (NDEA), N-nitrosodipropylamine (NDPA), N-nitrosodibutylamine (NDBA), N-nitrosopiperidine (NPIP), and N-nitrosopyrrolidine (NPYR) from salted aquatic products by gas chromatography-mass spectrometry (GC-MS). In this experiment, the separation and detection conditions were optimized for different extraction methods, solid-phase extraction columns, and chromatographic columns. The results showed that the linear correlation coefficients (R2) were higher than 0.9998 within 10-1000 μg/L, and the reproducibilities were good with the relative standard deviations (RSD) less than 8%. The recoveries were 79%-105%. It is noted that this method for the determination of volatile N-nitrosamine compounds in salted aquatic products was much more sensitivity and with a lower detection limits (0.05 μg/kg except NDPA) than the previously reported methods. This proposed method is rapid and convenient for the determination, and easy for the operation. It is appropriate for the determination of volatile N-nitrosamine compounds in various salted aquatic products.

Key words: N-nitrosamines, salted aquatic products, gas chromatography-mass spectrometry (GC-MS)