水产品中的亚硝胺前处理方法优化及4种N-亚硝胺类化合物快速检测

Optimization of Pretreatment Methods for Nitrosamines in Aquatic Products and Rapid Determination of Four Kinds of N-nitrosamine Compounds

该文采用改进的QuEChERS方法对水产样品进行提取、净化,建立气相色谱质谱联用快速检测N-亚硝胺类化合物的检测方法。样品经过乙腈和正己烷处理后,采用DB-WAX色谱柱分离并在质谱多反应监测模式下测定,采用外标法定量。4种N-亚硝胺类化合物在1.00μg/L~1000μg/L范围内线性关系良好,相关系数(r)>0.998。4类水产样品的水平加标回收率为89.0%~104.2%,相对标准偏差为0.6%~2.2%(n=6)。该方法操作简便,称样量少,试剂使用量少,前处理时间短,准确率高,能够满足水产品中N-亚硝胺类化合物的检测。

The improved QuEChERS(Quick,Easy,Cheap,Effective,Rugged,Safe)method was used to extract and purify aquatic samples,with the goal of establishing a rapid detection method for N-nitrosamine compounds by gas chromatography-mass spectrometry.Samples were treated with acetylene and positive hexane,and a DB-WAX column was used inthe multiple reaction monitoringmode to carry out the legal amount of the outer label.Four N-nitroamine compounds were isolated displayed good linear relationships ranging from 1.00μg/L to 1000μg/L[correlation coefficient(r)>0.998].The recoveries were 89.0%to 104.2%.The relative standard deviations were 0.6%to 2.2%(n=6).The improved QuEChERSmethod was simple to operate,required only small amounts of sample and reagent,had a short pre-processing time,and was very accurate.The improved method could detect N-nitrosamine compounds in aquatic products.