气相色谱-质谱法同时测定肉制品中9种N-亚硝胺的含量

摘要

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10~400 μg/L,线性相关系数达0.995 3以上,检出限 (LODs)低于0.04 μg/kg;在添加水平约为2.67 μg/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 10~400 μg/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 RSD of the samples are 82.64%~98.24% and 3.55%~5.98% respectively when the adding level is about 2.67 μg/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.