气相色谱-质谱法同时测定肉制品中9种N-亚硝胺的含量

Determination of Nine N-nitrosamines Content in Meat Products by GC-MS

为有效保障肉制品的食品安全,建立适用固相萃取-气相色谱-质谱（SPE-GC-MS）同时测定肉制品中N-二甲基亚硝胺（NDMA）、N-甲基乙基亚硝胺（NMEA）、N-二乙基亚硝胺（NDEA）、N-二丙基亚硝胺（NDPA）、N-二丁基亚硝胺（NDBA）、N-亚硝基哌啶（NPIP）、N-亚硝基吡咯（NPYR）、N-亚硝基吗啉（NMOR）及N-二苯基亚硝胺（NDPhA）等9种N-亚硝胺的方法,考察样品不同提取试剂、不同固相萃取小柱、不同色谱条件对分离检测的影响。结果表明：样品经过乙腈提取、固相萃取柱净化,采用GC-SIM-MS检测,外标法定量,在10-400μg/L,线性相关系数达0.995 3以上,检出限（LODs）低于0.04μg/kg;在添加水平约为2.67μg/kg时,该方法的平均回收率在82.64%-98.24%,相对标准偏差在3.55%-5.98%。该方法简便、快速,具有良好的灵敏度、重复性,可适用于同时测定肉制品中9种N-亚硝胺类化合物的含量。

Nine N-nitrosamines of NDMA,NMEA,NDEA,NDPA,NDBA,NPIP,NPYR,NMOR and NDPhA in meat products were detected simultaneously by the established suitable SPE-GC-MS to study the effect of different extract reagents,solid phase extraction column and chromatographic condition on separation determination of nine N-nitrosamines for effectively safeguarding food safety of meat products.Results：The linear correlation coefficient and detection limit of the samples within 10-400μg/L are above 0.995 3 and below 0.04 μg/kg after acetonitrile extraction,solid extraction column purification,GC-SIM-MS detection and external standard methods.The average recovery and RSDof the samples are 82.64%-98.24% and 3.55%-5.98% respectively when the adding level is about 2.67μg/kg.The established SPE-GC-MS method with advantages of simplicity,rapidity,good sensitivity and repetition should be used in simultaneous detection of nine N-nitrosamines content in meat products.