气相色谱-质谱联用法测定传统腌菜中的N-亚硝胺  

Determination of N-Nitrosamine Compounds in Traditional Pickled Vegetables by Gas Chromatography-Mass Spectrometry

作　　者：徐赛男[1] 吴祖芳[1] 陈杰[2] 

机构地区：[1]宁波大学海洋学院,浙江宁波315211 [2]宁波出入境检验检疫局,浙江宁波315012

出　　处：《食品与生物技术学报》2015年第11期1162-1167,共6页Journal of Food Science and Biotechnology

基　　金：国家自然科学基金项目(31171735);宁波市农业择优委托项目(2012C10016)

摘　　要：建立了气相色谱-质谱（GC-MS）快速测定腌制蔬菜中N-亚硝胺含量的分析方法。采用固相萃取（SPE）结合GC/MS检测了N-二甲基亚硝胺（NDMA）、N-二乙基亚硝胺（NDEA）,考察了样品不同提取方法、不同固相萃取洗脱剂配比对分离效果的影响。结果表明,固相萃取相较于超声萃取,回收率高且峰图干净,而固相萃取中选用90%的甲醇水溶液作为洗脱剂,不仅回收率均可达90%以上,同时也减少了有机溶剂的使用量,优化后两种N-亚硝胺的线性范围均为0.1-10.0 mg/L;相关系数分别达到0.994和0.999;检出限为0.02 mg/L;回收率为90%-112%;相对标准偏差（RSD）均小于2.3%,重现性良好。该方法前处理简便、快速,易于操作,适合各类腌制蔬菜中N-亚硝胺的检测。An analytical method was developed to determine the contents of N-nitrosamine compounds in pickled vegetables by solid-phase extraction（SPE） combining gas chromatography-mass spectrometry（GC-MS）. In this study,different extraction methods and the ratios of the eluents in SPE were investigated. The results showed that solid phase extraction got not only the higher recoveries but also the cleaner spectrum figure peaks compared with ultrasonic extraction. Moreover,by eluting with 90% methanol,the solid phase extraction obtained the recoveries more than 90% as well as reducing the organic solvent usage,the linear correlation coefficients of two N-nitrosamine compounds were up to 0.994 and 0.999 respectively,within0.1-10.0 mg/L. The detection limits were 0.02 mg/L and the recoveries were 90% -112%. The reproducibility was good with the relative standard deviations（RSD） less than 2.3%. This method is convenient and it is suitable for the determination of N-nitrosamine compounds in the pickled vegetables.

关 键 词：N-二甲基亚硝胺 N-二乙基亚硝胺 腌制蔬菜 固相萃取 气相色谱-质谱 

分 类 号：O657.63[理学—分析化学] TS255.53[理学—化学]