QuEChERS-气相色谱-串联质谱测定水产品中的12种拟除虫菊酯类农药

Determination of Twelve Pyrethroid Pesticides in Aquatic Products by QuEChERS-Gas Chromatography-Tandem Mass Spectrometry Method

建立了QuEChERS-气相色谱-串联质谱同时测定水产品中12种拟除虫菊酯类农药的检测方法。鱼、小龙虾样品经匀浆和QuEChERS前处理后即可进行气相色谱-串联质谱检测。12种拟除虫菊酯类农药在5~200μg/L浓度范围内线性良好,相关系数r 2≥0.9992,各组分的检出限(LOD)为3μg/kg,定量限(LOQ)为10μg/kg,满足国家标准(GB 31650-2021)限量值的分析要求。各组分在1LOQ、3LOQ、10LOQ的添加水平下,在鲫鱼、鳊鱼、草鱼和小龙虾中的回收率在81.5%~115.3%,相对标准偏差(RSD,n=3)均小于15%。本方法前处理简单高效,可用于水产品中12种拟除虫菊酯类农药的快速筛查。

A method for the determination of pyrethroid pesticides in aquatic products by QuEChERS-Gas chromatography-tandem mass spectrometry was established.Fishes and crawfish samples can be determinated by GC-MS/MS after being homogenated and pretreated by QuEChERS method.Twelve pyrethroid pesticides have a good linearship in the range of 5-200μg/L with r 2≥0.9992.The limits of detection(LODs)and limits of quantitation(LOQs)of each pesticide were 3μg/kg and 10μg/kg,respectively.At the spiked levels of 1 LOQ,3 LOQ and 10 LOQ,the recoveries of each pesticide ranged from 81.5%to 115.3%with RSDs<15%(n=3)in crucian carp,Chinese bream,grass carp and crawfish samples.The pretreatment of this method is simple and efficient,which can be used for rapid screening of 12 pyrethroid pesticides in aquatic products.