QuEChERS-气相色谱-串联质谱法测定熟肉制品中9种N-亚硝胺类化合物

Determination of nine N-nitrosamines in cooked meat by QuEChERS-gas chromatography-tandem mass spectrometry

目的建立同时测定熟肉制品中9种N-亚硝胺类化合物的气相色谱-串联质谱分析方法。方法样品采用快速基质分散净化(QuEChERS)法处理后,用HP-INNOWax石英毛细管色谱柱(30 m×0.25 mm,0.25μm)分离,经气相色谱-串联质谱多反应监测技术进行定性及定量分析。结果 9种N-亚硝胺类化合物在0.20～50.00μg/kg范围内线性关系良好,相关系数均>0.997,方法检出限为0.02～0.1μg/kg。3个加标水平的平均回收率为78%～120%,相对标准偏差为3.42%～15.24%。结论本方法准确、快速、灵敏度高,可用于熟肉制品中9种N-亚硝胺类化合物的检测。

Objective A method was established for simultaneous determination of nine N-nitrosamines in cooked meat using enhance matrix removal QuEChERS-gas chromatography-tandem mass spectrometry(GC-MS/MS).Methods The samples were extracted by enhance matrix removal QuEChERS.The analytes were separated on a HP-INNOWax quartz capillary column(30 m×0.25 mm,0.25μm),and ionized by electron impact ion source(EI).The data were collected by multiple reaction monitoring(MRM)mode,followed by qualitative screening and quantitative analysis.Results Nine N-nitrosamines had good linearities in the range of 0.20-50.00μg/kg,with correlation coefficients above 0.997.The detection limits of were 0.02-0.1μg/kg.The average recoveries of the nine N-nitrosamines were 78%-120%with relative standard deviations of 3.42%-15.24%.Conclusion The QuEChERS purification combined with GC-MS/MS method was rapid,accurate and sensitive,and suitable for the determination of nine N-nitrosamines in cooked meat.