固相萃取-在线凝胶渗透色谱-气相色谱质谱联用测定蔬菜干制品中的18种有机磷和拟除虫菊酯残留

Determination of 18 Organic Phosphorus and Pyrthroid Pesticides in Dried Vegetables using Solid-phase Extraction and On-line Gel Permeation Chromatography-GC/MS

摘要:

建立了蔬菜干制品中18种有机磷农药和拟除虫菊酯农药残留的在线凝胶渗透色谱-气相色谱/质谱（GPC-GC/MS）分析方法。样品以乙腈为提取剂超声波高速匀浆提取，提取液经ENVI-Carb固相萃取柱净化，除去样品中大部分的色素等干扰基质，再经在线GPC进一步净化除去大分子干扰物质，有效降低了样品基质带来的背景干扰。采用外标法定量，在质量浓度为0.02 mg/kg~0.5 mg/kg有良好的线性关系，加标水平为0.4 mg/kg时，18种农药的回收率基本都在80%~130%，相对标准偏差小于10%，检出限为0.001 mg/kg~0.026 mg/kg。经实验证明，该方法是一种快速，准确，灵敏度高的同时检测梅菜干中多种农药残留的检测方法。

Abstract:

An on-line gel permeation chromatography-GC/MS analytical method was developed for the determination of 18 organic phosphorus pesticide and pyrethroid pesticides in dried vegetables.The samples were extracted with acetonitrile by means of ultrasonic high-speed homogenization, cleaned up by an ENVI-Carb solid phase extraction column to remove pigment in the sample and analyzed by on-line gel permeation chromatography-GC/MS. All the compounds demonstrated good linear relationship in the range of 0.02~0.5 mg/kg. The recoveries for the most of pestive standards of 0.4 mg/kg were 80%-130% and the relative standard deviations were less than 10%. The limits of detection were from 0.001 mg/kg to 0.026 mg/kg. The method was rapid, accurate and highly sensitive, which can be used for the simultaneous determination of pesticide residues in dried vegetables.