QuEChERS结合大体积进样法测定水产干制品中N-二甲基亚硝胺  

Determination of N-dimethylnitrosamines in dried aquatic products by QuEChERS combined with a large volume injection method

作　　者：李湖平 王灵昭 钱亮亮 张建方 杜静 冯洪燕 盛世朵 张子岩 LI Hu-Ping;WANG Ling-Zhao;QIAN Liang-Liang;ZHANG Jian-Fang;DU Jing;FENG Hong-Yan;SHENG Shi-Duo;ZHANG Zi-Yan(College of Marine Food and Biological Engineering,Jiangsu Ocean University,Lianyungang 222005,China;Lianyungang Quality and Technology Comprehensive Inspection and Testing Center,Lianyungang 222006,China;Lianyungang Fangxin Food Co.,Ltd.,Lianyungang 222112,China)

机构地区：[1]江苏海洋大学海洋食品与生物工程学院,连云港222005 [2]连云港市质量技术综合检验检测中心,连云港222006 [3]连云港市方信食品有限公司,连云港222112

出　　处：《食品安全质量检测学报》2024年第4期210-217,共8页Journal of Food Safety and Quality

基　　金：连云港市重点研发计划(产业前瞻与关键核心技术科技项目)(CG2211)。

摘　　要：目的基于大体积进样(large-volume injections,LVI)系统建立QuEChERS结合气相色谱-串联三重四极杆质谱法测定水产干制品中N-二甲基亚硝胺化合物含量的分析方法。方法称取样品5 g,加5 mL水稀释后加入内标,经乙腈提取,提取液经PLS-A和ProElutQuE 15 mL Tube净化后,得到上机液。在多模式进样口(multi mode injection,MMI)中选择LVI模式进样,采用HP-INNOWAX石英毛细管柱(30 m×0.25 mm,0.25μm)分离,选择多反应监测(multiple reaction monitoring,MRM)模式进行测定,内标法定量。结果N-二甲基亚硝胺在0.1~20.0 ng/mL范围内呈现良好的线性关系,相关系数(r^(2))为0.9994,检出限为0.03μg/kg。在空白基质(不含N-二甲基亚硝胺化合物)样品中分别添加1、3、10μg/kg的3个水平混合标准溶液进行加标回收实验,加标回收率为85.7%~102.3%,相对标准偏差为3.6%~9.8%(n=6)。结论本法称样量少、有机试剂用量少、灵敏度高,能够满足水产干制品中N-二甲基亚硝胺含量的检测分析。Objective To establish a method for the determination of N-dimethylnitrosamine compounds in dried aquatic products by QuEChERS combined with gas chromatography-tandem triple quadrupole mass spectrometry(GC-MS/MS)based on large-volume injection(LVI)system.Methods The 5 g sample was weighed,diluted with 5 mL of water,then added to the internal standard,extracted by acetonitrile,and purified by PLS-A and ProElutQuE 15 mL Tube to obtain the upper solution.In the multi mode injection(MMI),the LVI mode was selected,the HP-INNOWAX quartz capillary column(30 m×0.25 mm,0.25μm)was used for separation,and the multiple reaction monitoring(MRM)mode was selected for measurement,and quantitative determination was performed by internal standard method.Results N-dimethylnitrosamine showed a good linear relationship in the range of 0.1-20.0 ng/mL,the correlation coefficient(r^(2))was 0.9994,the limit of detection was 0.03μg/kg.The 3 horizontal mixed standard solutions of 1,3 and 10μg/kg were added to the blank matrix(without N-dimethylnitrosamine compounds)for spiking recovery experiments,and the recoveries of spikes reached 85.7%-102.3%,and the relative standard deviations reached 3.6%-9.8%(n=6).ConclusionTThis method has a small sample size,a small amount of organic reagent and high sensitivity,which can meet the requirements for the detection and analysis of N-dimethylnitrosamine content in dried aquatic products.

关 键 词：N-二甲基亚硝胺 QUECHERS 气相色谱-串联三重四极杆质谱法 大体积进样 多反应监测 水产干制品 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]