GC-MS/MS测定水产品中的6种N-亚硝胺类化合物  

Determination of 6 N-nitrosamines in aquatic products by GC-MS/MS

作　　者：王玮 Stephan Altmaier Wei Wang;Stephan Altmaier(Merck Chemical Technology(Shanghai)Co.,LTD,Shanghai 200120,China;Merck Life Sciences KGaA,Darmstadt,Germany)

机构地区：[1]默克化工技术(上海)有限公司,上海200120 [2]Merck Life Sciences KGaA,Darmstadt,Germany

出　　处：《现代科学仪器》2024年第6期58-62,67,共6页Modern Scientific Instruments

摘　　要：建立气相色谱-串联质谱法(GC-MS/MS)分析水产品中6种N-亚硝胺类化合物(N-二甲基亚硝胺,N-甲基乙基亚硝胺,N-二乙基亚硝胺,N-二丙基亚硝胺,N-二丁基亚硝胺,N-亚硝基哌啶)的检测方法。样品经过乙腈提取,用基于QuEChERS原则的固相萃取法进行样品处理,最后乙腈定容,同时使用多模式进样口(MMI)溶剂放空模式直接进样5µL,GC-MS/MS多反应监测模式(MRM)测定,基质外标法定量。6种N-亚硝胺类化合物在0.1-10µg/L范围内呈现良好线性关系,相关系数均大于0.9990,在实际水产品的分析中,6种N-亚硝胺类化合物的加标回收率在82.9%-108%的范围内,相对标准偏差(RSD)为2.8-8.6%,方法检测限为0.05µg/L.该方法样品前处理简单、耗时短且灵敏度和回收率高,适用于分析水产品中的N-亚硝胺类化合物。To establish a gas chromatography-tandem mass spectrometry(GC-MS/MS)method for the determination of 6 N-nitrosamines(N-dimethylnitrosamines,n-methylethyl nitrosamines,n-diethylnitrosamines,n-dipropyl nitrosamines,n-dibutylnitrosamines,n-nitropiperidine)in aquatic products.The samples were extracted with acetonitrile and treated with QuEChERS principle based solid phase extraction method.Finally,the acetonitrile volume was fixed,and 5µL was directly injected with multi-mode inlet(MMI)solvent blowdown mode,determined by GC-MS/MS multi-reaction monitoring mode(MRM),and quantitative by matrix external standard method.The six N-nitrosamines showed a good linear relationship in the range of 0.1-10µg/L,and the correlation coefficients were all greater than 0.9990.In the analysis of actual aquatic products,the recoveries of the six N-nitrosamines were in the range of 82.9%to 108%,and the relative standard deviations(RSD)were 2.8-8.6%.The detection limit was 0.05µg/L.The method is simple,short in time,sensitive and high in recovery,and is suitable for the analysis of N-nitrosamines in aquatic products.

关 键 词：气相色谱-串联质谱法(GC-MS/MS) N-亚硝胺类化合物 多模式进样口(MMI) 

分 类 号：R284[医药卫生—中药学] O657.63[医药卫生—中医学]