陆正　陈红波　林刚健　方如意

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MgSO4和1 g NaCl作为脱水剂，经十八烷基键合硅胶（C18）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、20 μg/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。

关键词 QuEChERS-EMR;GC-MC;干制水产品;N-二甲基亚硝胺;含量测定

中图分类号 TS254.7文献标识码 A文章编号 0517-6611（2020）22-0181-04

doi：10.3969/j.issn.0517-6611.2020.22.048

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

LU Zheng， CHEN Hong-bo， LIN Gang-jian et al

（Taizhou Food Inspection and Testing Center，Taizhou，Zhengjing 318000）

Abstract [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 MgSO4 and 1 g of NaCl were used as dehydrating agents， purified by octadecyl bonded silica gel （C18）， 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， 20 μg/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.

Key words QuEChERS-EMR;GC-MC;Dried aquatic products;N-dimethylnitrosamine;Content determination

作者簡介 陆正（1994—），男，浙江台州人，助理工程师，从事食品检验检测工作。

收稿日期 2020-04-30;修回日期 2020-05-22

水产食品因低脂肪、高蛋白、营养均衡及味道鲜美等特点而受广大消费者的青睐，其中腌制手法通过抑制肉毒梭状芽孢杆菌及其他腐败菌的生长而提高水产品防腐性能、延长产品货架期，改善产品风味等特点作为水产品的最传统加工保藏方法[1-2]。相关研究结果表明，水产品腌制过程中所加入的硝酸盐和亚硝酸盐可与蛋白质生成胺反应，形成二甲基亚硝胺、吡咯亚硝胺等N-亚硝胺类化合物[3]，其中挥发性二甲基亚硝胺为最常见致癌物质。……