QuEChERS-EMR-GC/MS测定鱼肉制品中N-二甲基亚硝胺含量的方法学研究  

Methodological study on the determination of N-dimethyl nitrosamine in fish products by QuEChERS-EMR-GC/MS

作　　者：张洁 董榕贵 ZHANG Jie;DONG Ronggui(Guizhou Testing Technology Research and Application Center,Guiyang 550014,China)

机构地区：[1]贵州省检测技术研究应用中心,贵州贵阳550014

出　　处：《贵州科学》2024年第4期71-75,共5页Guizhou Science

摘　　要：目的:建立一种QuEChERS-EMR结合气相色谱串联质谱技术快速分析鱼肉制品中N-二甲基亚硝胺的方法。方法:样品加入内标,采用乙腈提取,经QuEChERS-EMR净化,VF-WaxMS(60 m×0.25 mm×0.25μm)色谱柱分离,在单离子检测(SIM)扫描,内标法定量。结果:N-二甲基亚硝胺在2.0~50.0 ng/mL浓度范围内线性关系良好,相关系数r为0.9994,方法检出限为1.0μg/kg,方法定量限为3.3μg/kg,添加浓度水平分别为4.0μg/kg、20μg/kg、40μg/kg时,测定回收率在83.1%~104.3%之间,相对标准偏差在3.3%~6.1%之间。鱼肉基质对N-二甲基亚硝胺的基质效应为7.5%,表现为弱基质效应,可以忽略。结论:该方法操作简便,经济高效,环保,准确度高和重复性好,以及基质效应弱,适用于鱼肉制品中N-二甲基亚硝胺的测定。In this study we established a method for the rapid analysis of N-dimethyl nitrosamine in fish products by QuEChERS-EMR-GC/MS.The internal standard was added to the sample,which was extracted with acetonitrile,purified with QuEChERS-EMR,separated by VF-WaxMS column(60 m×0.25 mm×0.25μm),scanned under single ion detection(SIM)mode,and quantified by internal standard method.N-dimethyl nitrosamine had good linear relationship within the concentration range of 2.0 ng/mL to 50.0 ng/mL,and the correlation coefficient was 0.9994.The limit of detection was 1.0μg/kg,and the limit of quantitation was 3.0μg/kg.The recoveries were between 83.1%and 104.3%when the spiked levels were 4.0μg/kg,20μg/kg and 40μg/kg.The relative standard deviation was between 3.3%and 6.1%.The matrix effect of fish substrate on N-dimethyl nitrosamine was 7.5%,showing a weak matrix effect and could be ignored.The method is simple,efficient and environmental protective,with high accuracy and good repeatability,which is suitable for the determination of N-dimethyl nitrosamine in fish products.

关 键 词：QuEChERS-EMR N-二甲基亚硝胺 鱼肉制品 气相色谱串联质谱 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]