分析化学2013，Vol.41Issue(7)：1044-1049,6.DOI:10.3724/SP.J.1096.2013.21193
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
摘要
Abstract
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,C18,Silica,and Diatomite) and two SPE columns with mixed dual packing materials (Al2O3-C18,Al2O3-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 mg/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Key words
N-nitrosamines/ High performance liquid chromatography/ Mass spectrometry/ Solid phase extraction on dual packing materials column/ Pickled vegetables引用本文复制引用
杨宁,陈颖慧,邓莉,邝敏杰,段李歌,刘志伟,何静仁..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[J].分析化学,2013,41(7):1044-1049,6.基金项目
本文系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) （No.D20121803）
武汉工业学院2011年研究生创新基金项目(No.2011cx017)资助 （No.2011cx017）
