气相色谱法测定坚果中16种有机氯、拟除虫菊酯类农药残留量
Determination of 16 Kinds of Organochlorine and Pyrethroid Pesticide Residues in Nuts by Gas Chromatography
李娜 1朱文峰 1程国栋 1江婷婷 1王婷 1冀常菲1
作者信息
- 1. 安徽中创食品检测有限公司,安徽芜湖 241000
- 折叠
摘要
建立气相色谱法(gas chromatography,GC)检测坚果中 16种有机氯、拟除虫菊酯类农药残留的分析方法.样品通过丙酮:正己烷(3:7,V:V)提取,0.2 mL浓硫酸磺化净化,有机氯和拟除虫菊酯经DB-17MS色谱柱(30 m×0.32 mm,0.25 μm)分离,气相色谱-电子捕获检测器(gas chromatography-electron capture detector,GC-ECD)定量检测.有机氯、拟除虫菊酯类农药在0.01～0.20 μg/mL浓度范围内与对应的峰面积呈现良好的线性关系,决定系数(r2)均在 0.996以上,方法检出限为 0.1～0.4 μg/kg;分别对不同基质(开心果、澳洲坚果、腰果、碧根果、核桃、巴旦木)样品进行低(10 μg/kg)、中(40 μg/kg)、高(100 μg/kg)3个浓度加标提取率实验,提取率范围为 81.6%～119.5%,相对标准偏差(relative standard deviation,RSDs)为 1.03%～5.36%.本方法分析简单、准确度高、重复性好,适用于坚果中16种有机氯、拟除虫菊酯类农药残留的测定.
Abstract
The purpose of this paper is to establish an analytical method for the determination of 16 organochlorine and pyrethroid pesticide residues in nuts by gas chromatography(GC).The samples were extracted by acetone:hexane(3:7,V:V),purified by 0.2 mL concentrated sulfuric acid sulfonation,and the organochlorines and pyrethroids were separated by a DB-17MS column(30 m×0.32 mm,0.25 μm),and quantified by gas chromatography-electron capture detector(GC-ECD).The results showed that the organochlorine and pyrethroid pesticides showed good linearity in the concentration range of 0.01～0.20 μg/mL and the corresponding peak areas.The determination coefficients(r2)were above 0.996,and the limits of detection were 0.1～0.4 μg/kg.In this study,the spiked recovery experiments were also performed on samples of different matrices(pistachios,macadamia nuts,cashew nuts,pistachios,walnuts,and padanuts)at low(10 μg/kg),medium(40 μg/kg),and high(100 μg/kg)concentrations,respectively.The extraction rates ranged from 81.6%to 119.5%with the relative standard deviations(RSDs)of 1.03%～5.36%.The method is simple,accurate,reproducible and suitable for the determination of 16 organochlorine and pyrethroid pesticide residues in nuts.
关键词
坚果/有机氯/拟除虫菊酯类/浓硫酸磺化/气相色谱法Key words
nuts/organochlorine/pyrethroid/concentrated sulfuric acid sulfonation/gas chromatography引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
维普
万方数据