气相色谱—串联质谱法快速测定禽蛋中203种农药及化学污染物残留
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摘要
随着经济发展和人们生活水平的不断提高,人们对食品安全问题越来越重视。农药对食品的污染是影响食品安全的主要因素,也是各国衡量食品卫生和质量安全的首要指标。同时,世界各国在食品进出口方面对农药残留的要求越来越严格,因此建立快速、简单、准确的农药检测方法是保证食品安全的首要任务。本文初步建立了气相色谱-串联质谱法测定禽蛋中农药及化学污染物残留的分析方法。全文共分为2章：
第1章本章介绍了农药、农药的分类、农药的中毒机理和农药残留及其对人体健康的危害。重点综述了食品农残常用的前处理技术、检测方法及其原理和应用。
第2章本章主要阐述了气相色谱-串联质谱法快速测定禽蛋中203种农药以及化学污染物残留。比较了4种除水实验方案、8种提取溶剂、9种净化固相萃取柱(包括SPE柱对农药的吸附实验,SPE柱的净化效果实验以及SPE柱对农药的回收率实验)以及5种洗脱溶剂对样品的提取净化效果。最终确定了用15mL乙腈提取,C18+Carb串联固相萃取柱净化,20mL乙腈-甲苯(3:1,v/v)洗脱,GC-MS/MS检测的实验方法。本方法的检出限为0.03μg/kg 181.9μg/kg,其回收率在60%～120%的有183种,占研究总数的90.1%；相对标准偏差<20%的有197种,占研究总数的97.0%。
With economic development and continuous improvement of living standards, people pay more and more attention to food safety issues. Pesticide contamination of food is not only the main factor affecting food security, but also the primary indicator for many countries to measure the quality of food hygiene and safety. At the same time, more and more strict requirements have been put on the pesticide residues in food import and export, so establishing a rapid, simple and accurate detection of pesticides is the primary task of ensuring food safety. In this thesis, a gas chromatography - tandem mass spectrometry method has been established for the analysis of 203 kinds of pesticide residues in eggs. The thesis is divided into two chapters:
Chapter 1 This chapter describes pesticide classification, mechanism of pesticide poisoning and pesticide residues and pesticide residues on human health hazards. Commonly used sample preparation methods and detection methods for the analysis of pesticide residues in food are reviewed.
Chapter 2 This chapter describes the gas chromatography tandem mass spectrometry method for the rapid detection of 203 species of pesticide residues in eggs. This paper compares the effects of four water-removing methods,8 kinds of extraction solvents,9 kinds of solid phase extraction columns (including the SPE column adsorption experiments of pesticides, SPE column purification experiments and the recovery of pesticides experiments), and 5 kinds of eluting solvents.The optimized extraction and purification conditions are as follows:the sample was extracted with 15 mL acetonitrile, purified by C18+Carb solid phase extraction cartridges and eluted with 20 mL of acetonitrile:toluene (3:1, v/v).The detection limits were in the range of 0.03μg/kg-181.9μg/ kg, the recoveries were between 60% and 120% for 183 species of pesticides, accounting for 90.1% of the total number of pesticides; the relative standard deviation<20% for 197 species, accounting for 97.0% of the total number of pesticides.
第1章本章介绍了农药、农药的分类、农药的中毒机理和农药残留及其对人体健康的危害。重点综述了食品农残常用的前处理技术、检测方法及其原理和应用。
第2章本章主要阐述了气相色谱-串联质谱法快速测定禽蛋中203种农药以及化学污染物残留。比较了4种除水实验方案、8种提取溶剂、9种净化固相萃取柱(包括SPE柱对农药的吸附实验,SPE柱的净化效果实验以及SPE柱对农药的回收率实验)以及5种洗脱溶剂对样品的提取净化效果。最终确定了用15mL乙腈提取,C18+Carb串联固相萃取柱净化,20mL乙腈-甲苯(3:1,v/v)洗脱,GC-MS/MS检测的实验方法。本方法的检出限为0.03μg/kg 181.9μg/kg,其回收率在60%～120%的有183种,占研究总数的90.1%；相对标准偏差<20%的有197种,占研究总数的97.0%。
With economic development and continuous improvement of living standards, people pay more and more attention to food safety issues. Pesticide contamination of food is not only the main factor affecting food security, but also the primary indicator for many countries to measure the quality of food hygiene and safety. At the same time, more and more strict requirements have been put on the pesticide residues in food import and export, so establishing a rapid, simple and accurate detection of pesticides is the primary task of ensuring food safety. In this thesis, a gas chromatography - tandem mass spectrometry method has been established for the analysis of 203 kinds of pesticide residues in eggs. The thesis is divided into two chapters:
Chapter 1 This chapter describes pesticide classification, mechanism of pesticide poisoning and pesticide residues and pesticide residues on human health hazards. Commonly used sample preparation methods and detection methods for the analysis of pesticide residues in food are reviewed.
Chapter 2 This chapter describes the gas chromatography tandem mass spectrometry method for the rapid detection of 203 species of pesticide residues in eggs. This paper compares the effects of four water-removing methods,8 kinds of extraction solvents,9 kinds of solid phase extraction columns (including the SPE column adsorption experiments of pesticides, SPE column purification experiments and the recovery of pesticides experiments), and 5 kinds of eluting solvents.The optimized extraction and purification conditions are as follows:the sample was extracted with 15 mL acetonitrile, purified by C18+Carb solid phase extraction cartridges and eluted with 20 mL of acetonitrile:toluene (3:1, v/v).The detection limits were in the range of 0.03μg/kg-181.9μg/ kg, the recoveries were between 60% and 120% for 183 species of pesticides, accounting for 90.1% of the total number of pesticides; the relative standard deviation<20% for 197 species, accounting for 97.0% of the total number of pesticides.
引文
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