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

中文关键词:  N-二甲基亚硝胺  QuEChERS  三重四极杆气质联用仪  大体积进样  多反应监测

英文关键词:N-dimethylnitrosamine  QuEChERS  gas chromatography-tandem triple quadrupole mass spectrometry  large-volume injection  multiple reaction monitoring  dried aquatic products

中文摘要:

      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 15mL 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, HP-INNOWAX石英毛细管柱分离, 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(r2)为0.9994,检出限为0.03 μg/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、10 μg/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。

英文摘要:

      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 sample was weighed 5 g, diluted with 5 mL of water, 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 was separated, and the multiple reaction monitoring (MRM) mode was selected for measurement, and the internal standard method was quantified. Results N-dimethylnitrosamine showed a good linear relationship in the range of 0.1~20.0 ng/mL, the correlation coefficient (r2) was 0.9994, the detection limit was 0.03 μg/kg. The three horizontal mixed standard solutions of 1, 3 and 10 μg/kg were added to the blank matrix (without N-dimethylnitrosamine compounds) for spiking recovery experiments, and the recoveryrate of spikes reached 85.7%~102.3%, and the relative standard deviationreached 3.6%~9.8% (n=6). Conclusion This 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.