色质联用技术在坚果中农药多残留分析中的应用
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摘要
农药残留是影响食品质量和安全的重要问题之一,已经引起世界各国政府和组织的高度关注,也是国际贸易中高度关注的重要问题。所以,发展准确、快速、灵敏和实用的农药残留分析技术无疑是控制农药残留、保证食品安全和保障我国食品进出口的基础。本文采用气相色谱-串联质谱联用技术,选择有限量要求的185种农药做检测,优化了坚果类食品农药残留检测的各种条件,建立了一种简单、准确、检出限低、检测农药种类全的确证方法。全文共分2章:
第1章在参考124篇文献的基础上,综述了检测农药残留常用的样品前处理方法和检测方法。样品前处理方法介绍了固相萃取法、固相微萃取、凝胶渗透色谱法、超临界流体萃取、基质固相分散萃取、加速溶剂萃取和微波辅助萃取技术。检测方法介绍了酶抑制法、免疫分析法、生物传感器法和色谱法。
第2章建立了坚果(花生仁、葵花籽、核桃仁和杏仁)中185种农药的气相色谱-串联质谱(GC-MS/MS)检测方法。样品经含1%乙酸的乙腈提取、C18串联PSA固相萃取柱净化,气相色谱-串联质谱测定。185种农药在坚果样品中的检出限(S /N = 5 )范围是0.02μg/kg～526.4μg/kg,其中10μg/kg以下的农药数目占到检测农药总数的81%,185种农药的定量限(LOQ)均低于最大残留限量(MRLs)。185种农药在1倍LOQ～83倍LOQ浓度范围内线性关系良好(r > 0.99)。以定量限(LOQ)、2倍定量限(2LOQ)、4倍定量限(4LOQ)三个浓度添加水平对四种坚果类样品进行了添加回收实验,86.0%的农药平均回收率在70%～110%之间;90.5%的农药平均回收率为60%～120%;82.3%的农药回收率的相对标准偏差(RSD)小于10%。方法准确、灵敏、简便,可用于坚果中农药残留的日常检测。
Pesticide residue is one of the important issues that affect food quality and safety .It has attracted the great concern of the world's governments and organizations and is a greatly concerned and important issue in international trade. Therefore, the development of accurate, rapid, sensitive and practical method for the analysis of pesticide residues is undoubtedly the basis of controling pesticide residues, guaranteeing food safety and ensuring food import and export. In this paper, Gas chromatography - tandem mass spectrometry was employed to detect 185 kinds of pesticides having MRL in nuts. The detcetion conditions were optimized and the established method was proved to be simple and accurate with low detection limit. This thesis is divided into two chapters:
Chapter 1, Based on 124 papers, commonly used sample preparation and detection methods for the analysis of pesticide residues were reviewed. Among sample preparation methods, solid phase extraction, solid phase micro extraction, gel permeation chromatography, supercritical fluid extraction, matrix solid phase dispersion extraction, accelerated solvent extraction and microwave assisted extraction were discussed. Among detection methods, enzyme inhibition, immunoassay, biosensors and chromatography were introduced.
Chapter 2, A method was developed for the determination of 185 pesticides in nuts(Peanuts, Sunflower seeds, Walnuts and Almonds )by gas chromatography tandem mass spectrometry (GC-MS/MS) .The sample was extracted by 1% acetic acid acetonitrile and cleaned up by C18 tandem PSA solid-phase extraction. Detection limits (S /N = 5) ranged from 0.02 to 526.4μg/kg, and 81% pesticides were found to be below 10μg/kg,and all LOQ(limit of quantification) of these 185 pesticides were less than the maximum residue limits (MRL).These 185 pesticides have shown a good linear relationship with correlation coefficients larger than 0.99 ranged from LOQ to 83 LOQ. The recoveries were determined at three spiked levels of 1 LOQ ,2 LOQ and 4 LOQ in four samples. The average recoveries of 86.0% pesticides were between 70% and 110%; 90.5% pesticides were between 60% and 120%.RSDs of 82.3% pesticides were less than 10%. The established method is accurate,sensitive and simple,and can be used for the routine analysis of pesticide residues in nuts .
第1章在参考124篇文献的基础上,综述了检测农药残留常用的样品前处理方法和检测方法。样品前处理方法介绍了固相萃取法、固相微萃取、凝胶渗透色谱法、超临界流体萃取、基质固相分散萃取、加速溶剂萃取和微波辅助萃取技术。检测方法介绍了酶抑制法、免疫分析法、生物传感器法和色谱法。
第2章建立了坚果(花生仁、葵花籽、核桃仁和杏仁)中185种农药的气相色谱-串联质谱(GC-MS/MS)检测方法。样品经含1%乙酸的乙腈提取、C18串联PSA固相萃取柱净化,气相色谱-串联质谱测定。185种农药在坚果样品中的检出限(S /N = 5 )范围是0.02μg/kg～526.4μg/kg,其中10μg/kg以下的农药数目占到检测农药总数的81%,185种农药的定量限(LOQ)均低于最大残留限量(MRLs)。185种农药在1倍LOQ～83倍LOQ浓度范围内线性关系良好(r > 0.99)。以定量限(LOQ)、2倍定量限(2LOQ)、4倍定量限(4LOQ)三个浓度添加水平对四种坚果类样品进行了添加回收实验,86.0%的农药平均回收率在70%～110%之间;90.5%的农药平均回收率为60%～120%;82.3%的农药回收率的相对标准偏差(RSD)小于10%。方法准确、灵敏、简便,可用于坚果中农药残留的日常检测。
Pesticide residue is one of the important issues that affect food quality and safety .It has attracted the great concern of the world's governments and organizations and is a greatly concerned and important issue in international trade. Therefore, the development of accurate, rapid, sensitive and practical method for the analysis of pesticide residues is undoubtedly the basis of controling pesticide residues, guaranteeing food safety and ensuring food import and export. In this paper, Gas chromatography - tandem mass spectrometry was employed to detect 185 kinds of pesticides having MRL in nuts. The detcetion conditions were optimized and the established method was proved to be simple and accurate with low detection limit. This thesis is divided into two chapters:
Chapter 1, Based on 124 papers, commonly used sample preparation and detection methods for the analysis of pesticide residues were reviewed. Among sample preparation methods, solid phase extraction, solid phase micro extraction, gel permeation chromatography, supercritical fluid extraction, matrix solid phase dispersion extraction, accelerated solvent extraction and microwave assisted extraction were discussed. Among detection methods, enzyme inhibition, immunoassay, biosensors and chromatography were introduced.
Chapter 2, A method was developed for the determination of 185 pesticides in nuts(Peanuts, Sunflower seeds, Walnuts and Almonds )by gas chromatography tandem mass spectrometry (GC-MS/MS) .The sample was extracted by 1% acetic acid acetonitrile and cleaned up by C18 tandem PSA solid-phase extraction. Detection limits (S /N = 5) ranged from 0.02 to 526.4μg/kg, and 81% pesticides were found to be below 10μg/kg,and all LOQ(limit of quantification) of these 185 pesticides were less than the maximum residue limits (MRL).These 185 pesticides have shown a good linear relationship with correlation coefficients larger than 0.99 ranged from LOQ to 83 LOQ. The recoveries were determined at three spiked levels of 1 LOQ ,2 LOQ and 4 LOQ in four samples. The average recoveries of 86.0% pesticides were between 70% and 110%; 90.5% pesticides were between 60% and 120%.RSDs of 82.3% pesticides were less than 10%. The established method is accurate,sensitive and simple,and can be used for the routine analysis of pesticide residues in nuts .
引文
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