QuEChERS-EMR结合GC-MS检测干制水产品中N-二甲基亚硝胺含量  

Detection of N-dimethylnitrosamine in Dried Aquatic Products by QuEChERS-EMR Combined with GC-MS

作　　者：陆正 陈红波 林刚健 方如意 LU Zheng;CHEN Hong-bo;LIN Gang-jian(Taizhou Food Inspection and Testing Center,Taizhou,Zhengjing 318000)

机构地区：[1]台州市食品检验检测中心,浙江台州318000

出　　处：《安徽农业科学》2020年第22期181-184,共4页Journal of Anhui Agricultural Sciences

摘　　要：[目的]采用QuEChERS结合气相色谱-质谱联用技术建立检测水产干制品中N-二甲基亚硝胺的高效且准确性高的方法。[方法]通过预处理制备条件优化即样品采用乙腈进行提取,利用4 g无水MgSO 4和1 g NaCl作为脱水剂,经十八烷基键合硅胶(C 18)净化,并通过提取后添加的方法进行基质效应评估。[结果]N-二甲基亚硝胺标准曲线的线性相关系数大于0.99,通过基质匹配绘制标准曲线后能较好地消除基质效应的影响,从而提高定量分析检测的准确度;通过N-二甲基亚硝胺在水产品基质加标3水平(5、10、20μg/kg)的平均回收率为79.8%~102.1%,相对偏差均小于10%。[结论]该试验方法具有前处理简单、用量少、耗时短、准确性较高等特点,能满足水产品中N-二甲基亚硝胺检测的要求。[Objective]An efficient and accurate method for the detection of N-dimethylnitrosamines in dried aquatic products was developed using QuEChERS combined with gas chromatography-mass spectrometry.[Method]The pre-treatment conditions were optimized,that was,the sample was extracted with acetonitrile,4 g of anhydrous MgSO 4 and 1 g of NaCl were used as dehydrating agents,purified by octadecyl bonded silica gel(C 18),and matrix effect was evaluated by the method after extraction.[Result]The linear correlation coefficient of the standard curve of N-dimethylnitrosamine was greater than 0.99.The matrix effect could be eliminated by drawing a standard curve through matrix matching,thereby improving the accuracy of quantitative analysis and detection;the average recovery of three levels(5,10,20μg/kg)of N-dimethylnitrosamine in the aquatic product matrix was 79.8%-102.1%,the relative deviations were less than 10%.[Conclusion]This test method has the characteristics of simple pretreatment,small amount,short time-consuming and high accuracy,and can meet the requirements for the detection of N-dimethylnitrosamines in aquatic products.

关 键 词：QuEChERS-EMR GC-MC 干制水产品 N-二甲基亚硝胺 含量测定 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]