双填料固相萃取-高效液相色谱/质谱法同时检测腌菜中9种N-亚硝胺  

Simultaneous Determination of Nine Nitrosamines in Pickled Vegalables by Solid Phase Extration Column of Dual Packing Materials and HPLC/MS

作　　者：杨宁[1] 陈颖慧[1,2] 邓莉[1] 邝敏杰[1] 段李歌[1] 刘志伟[1] 何静仁[1] 

机构地区：[1]湖北省农产品加工与转化重点实验室武汉工业学院食品科学与工程学院,武汉430023 [2]中央储备粮麻城直属库,麻城438300

出　　处：《分析化学》2013年第7期1044-1049,共6页Chinese Journal of Analytical Chemistry

基　　金：湖北省教育厅科学技术研究重点项目(No.D20121803);湖北省政府楚天学者计划(2012);武汉工业学院2011年研究生创新基金项目(No.2011cx017)资助

摘　　要：亚硝胺是三大强致癌食品污染物之一,普遍存在于腌制和热加工食品中。本研究建立了一种基于液质联用技术结合多级反应监测模式扫描(MRM)检测N-亚硝胺的新型固相萃取-液相色谱方法,可以快速直接检测腌菜中9种N-亚硝胺。实验优化了液相色谱分离与检测条件,同时考察了4种固相萃取单柱(碱性氧化铝Al2O3、C18、硅胶、硅藻土)和2种双填料的混合固相萃取柱(Al2O3-C18,Al2O3-硅胶)吸附解析的净化效果。结果表明,采用Al2O3-C18混合柱纯化,液相色谱检测,外标法定量,对9种亚硝胺的回收率达75.7%～116.0%,检出限为0.20～0.49 mg/L。采用本方法检测不同产地的6类腌菜产品中亚硝胺含量,二甲基亚硝胺和二乙基亚硝胺的检出率相对较高,分别为37.5%和25.0%,其中二乙基亚硝胺在雪里蕻腌菜中最高含量达59.1 mg/L,亚硝基吗啉在所有样品中未检出。Nitrosamine is one of the three strong carcinogenic contaminants in food and widely present in pickled and heat-treated food. A new solid phase extraction （SPE）-HPLC method based on the HPLC-MS identification for the determination of nine nitrosamines has been established. The method could be used for the direct and fast detection of 9 nitrosamines in pickles. The conditions for chromatographic separation and detection have been optimized. Four SPE columns with single packing materials （Al2O3, Cls, Silica, and Diatomite） and two SPE columns with mixed dual packing materials （Al2O3-C18, Al/O3-Silica） have also been investigated. As a result, the recoveries for determination of 9 nitrosamines by HPLC with SPE column of mixed Al2O3-C18 for cleanup were in the range of 75.7% to 116.0% and the limit of detection was 0.20- 0.49 mg/L. On the basis of the above methods, the concentrations of nitrosamines in pickled vegetables of six varieties produced from different origins were investigated. The occurrence rate of N-nitrosodiethylamine （NDMA） and NDEA in all samples was 37.5% and 25.0%, relatively higher than that of other nitrosamines. The highest content of NDEA occurred especially in potherb mustard was up to 59. 1 rag/L, and N-nitrosomorpholine （NMOR） has not been detected in all samples.

关 键 词：N-亚硝胺 液相色谱 质谱 双填料固相萃取 腌菜 

分 类 号：TS255.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]