茶葉農藥多殘留檢測方法學研究

《茶葉農藥多殘留檢測方法學研究》是2019年10月出版的圖書，作者是龐國芳。

基本信息

茶葉農藥多殘留檢測方法學研究（Analysis of Pesticide in Tea：Chromatography-Mass Spectrometry Methodology）

所屬類別

科技 >> 化學 >> 分析科學與技術

作者：龐國芳 著

出版日期：2019年10月

書號：978-7-122-34411-3

開本：大16K　889×1194　1/16

裝幀：精

版次：1版1次

頁數：887頁

內容簡介

本書詳細介紹了一系列測定茶葉中農藥殘留的快速高通量分析方法，具有高精度、高可靠性、高靈敏度的特點，適用廣泛。全書共7章：茶葉農藥殘留分析基礎研究和檢測方法建立；不同樣品製備技術提取淨化效能對比研究；茶葉水化對農藥多殘留方法效率的影響；茶葉農藥殘留測定基質效應及其補償作用研究；方法耐用性系統評價，誤差原因分析，關鍵控制點建立；茶葉陳化樣品和污染樣品農藥降解規律研究；經11個國家和地區的30個實驗室國際協同研究，建立茶葉中653種農藥化學污染物高通量分析方法AOAC標準。

本書可作為科研單位、高等院校、質檢機構等各類專業技術人員從事食品安全、環境保護、農業科技及農藥開發等技術研究與套用的參考書，也可作為大學教學參考書。

圖書目錄

Preface xi

Introduction xiii

1 Fundamental Research: Analytical

Methods for Multiresidues in Tea

1.1 Simultaneous Determination of 653

Pesticide Residues in Teas by Solid

Phase Extraction (SPE) with Gas

Chromatography–Mass Spectrometry

(GC–MS) and Liquid Chromatography–

Tandem Mass Spectrometry

(LC–MS/MS) 3

1.1.1 Introduction 3

1.1.2 Experimental 4

1.1.2.1 Reagents and Materials 4

1.1.2.2 Apparatus 5

1.1.2.3 Extraction 5

1.1.2.4 Cleanup 5

1.1.2.5 Determination 5

1.1.3 Results and Discussion 6

1.1.3.1 Optimization of Gas

Chromatography–Mass Spectrometry

Conditions and Selection of Pesticide

Varieties Suitable for Analysis 6

1.1.3.2 Optimization of Liquid

Chromatography–Tandem Mass

Spectrometry Conditions and

Selection of Pesticide Varieties

Suitable for Analysis 6

1.1.3.3 Optimization of Sample Extraction

Conditions 10

1.1.3.4 Optimization of Sample Cleanup

Conditions 12

1.1.3.5 Evaluation of Method Effi ciency—

LOD, LOQ, Recovery and Relative

Standard Deviations of Both Gas

Chromatography–Mass Spectrometry

and Liquid Chromatography–Tandem

Mass Spectrometry 48

References 90

1.2 Research on the Evaluation of the

Effectiveness of the Nontargeting,

High-Throughput Method for the

Detection of 494 Pesticides Residue

Using GC-Q-TOF/MS Technique

in Tea 91

1.2.1 Introduction 91

1.2.2 Experimental 92

1.2.2.1 Reagents, Standard, and Materials 92

1.2.2.2 Equipment 93

1.2.2.3 Condition of Gas Chromatography and Mass Spectrometry 93

1.2.2.4 Pretreatment Methods for the Screening Analysis of Tea Samples 93

1.2.3 Establishment of Database 93

1.2.4 Evaluation of the Effi ciency of the Method 93

1.2.4.1 Qualitative Analysis 94

1.2.4.2 Screening Limit 95

1.2.4.3 Recovery (Rec. 60%–120%&RSD < 20%) 111

1.2.4.4 Comprehensive Analysis

(Comparative Analysis the Infl uence

of Matrix on the Screening Limit

and Recovery of Pesticides) 113

1.2.5 Conclusion 114

1.3 A Study of Effi ciency Evaluation for

Nontarget and High-Throughput

Screening of 556 Pesticides Residues

by LC-Q-TOF/MS 115

1.3.1 Introduction 115

1.3.2 Experimental 116

1.3.2.1 Reagents and Materials 116

1.3.2.2 HPLC Conditions 116

1.3.2.3 Mass Spectrometry Conditions 116

1.3.2.4 Sample Preparation 117

1.3.3 Creation of the Pesticide Database 117

1.3.4 Method Evaluation 117

1.3.4.1 Qualitative Analysis 117

1.3.4.2 Screening Limits 117

1.3.4.3 Accuracy and Precision 119

1.3.4.4 Comprehensive Analysis of Screening Limits and Recoveries 124

1.3.5 Conclusions 124

1.4 A Study of Effi ciency Evaluation for

Nontarget Screening of 1050 Pesticide

By TOFMS and

LC–Q–TOF/MS 143

1.4.1 Introduction 143

1.4.2 Experimental 143

1.4.2.1 Reagents and Materials 143

1.4.2.2 Standard Solution Preparation 144

1.4.2.3 Sample Collection and Pretreatment 144

1.4.2.4 Instrumental Analysis 144

1.4.2.5 Creation of the Pesticides Database 144

1.4.2.6 Method Evaluation 145

1.4.3 Results and Discussion 145

1.4.3.1 Screening Limits Analysis 145

1.4.3.2 Accuracy and Precision 147

1.4.3.3 Comparison of the Common-Detected Pesticides 150

1.4.4 Conclusion 152

2 Comparative Study of Extraction

and Cleanup Efficiencies of Residue

Pesticides in Tea

2.1 Review of Sample Preparation

Techniques for Residue Pesticides

in Tea 223

2.1.1 Review of Solid Phase Extraction Technique 223

2.1.2 Review of QuEChERS Method 224

References 225

2.2 Comparative Study of Extraction

Effi ciencies of the Three Sample

Preparation Techniques 227

2.2.1 Introduction 227

2.2.2 Experimental 228

2.2.2.1 Reagents and Materials 228

2.2.2.2 Apparatus 228

2.2.2.3 Experimental Method 228

2.2.3 Preparing Pesticides Incurred Tea

Samples and Deciding the Precipitated

Content of the Target Pesticide 229

2.2.4 Optimization of Experimental Conditions for Method-3 229

2.2.5 Optimization of the Evaporation

Temperatures and Degrees of the

Sample Solutions for Three Methods 245

2.2.5.1 Optimization Selection

of Temperatures of Rotary

Evaporation 245

2.2.5.2 Optimum Selection of the Degree of Rotary Evaporation 245

2.2.6 Stage I: Evaluation on the Extraction

Effi ciencies of the Multiresidue

Pesticides in Green Tea Samples

by Method-1, Method-2, and

Method-3 246

2.2.6.1 Test Data Analysis 246

2.2.6.2 Analysis of Experimental Phenomenon 246

2.2.7 Stage II: Evaluation on the Extraction

Effi ciencies of the Multiresidue

Pesticides in Green Tea and Oolong

Tea Samples by Method-1 and

Method-2 256

2.2.8 Stage III: Evaluation on the Extraction

Effi ciencies of Green Tea and Oolong

Tea Sample the Incurred 201 Pesticides

After 165 days by Method-1 and

Method-2 266

2.2.8.1 Test Data Analysis 266

2.2.8.2 Test Phenomenon Analysis 266

2.2.9 Conclusions 277

2.3 The Evaluation of the Cleanup

Effi ciency of SPE Cartridge Newly

Developed for Multiresidues

in Tea 279

2.3.1 Introduction 279

2.3.2 Reagents and Materials 280

2.3.3 Apparatus 280

2.3.4 Experimental 280

2.3.5 Stage I: The Comparative Test of the

Cleanup Effi ciencies of 12 SPE

Combined Cleanup Cartridges

Against the Spiked 84 Pesticides

in Tea 280

2.3.6 Stage II: The Comparative Test on

Cleanup Effi ciencies of Spiked 201

Pesticides in Tea with 4# Envi-Carb+PSA

Tandem Cartridge and Cleanert TPT 281

2.3.7 Stage III: The Comparative Test on the

Cleanup Efficiencies of Green Tea and

Oolong Tea Youden Pair Samples

Incurred by 201 Pesticides with

Cleanert TPT Cartridge and 4# Envi-

Carb+PSA Combined Cartridge 287

2.3.7.1 Comparison of the Determined

Values of Target Pesticide

Content 287

2.3.7.2 Comparison of the Reproducibility

of the Target Pesticide

Determination 295

2.3.8 Conclusions 329

References 464

3 Study on the Influences of Tea

Hydration for the Method Efficiency

and Uncertainty Evaluation of

the Determination of Pesticide

Multiresidues in Tea Using Three

Sample Preparation Methods/

GC–MS/MS

3.1 A Comparative Study on the Influences

of Tea Hydration for the Method

Efficiency of Pesticide Multiresidues

Using Three Sample Preparation

Methods/GC–MS/MS 467

3.1.1 Introduction 467

3.1.2 Experimental Method 469

3.1.2.1 Three Different Sample Preparation Methods 469

3.1.2.2 Aged Sample Preparation 469

3.1.2.3 Incurred Sample Preparation 469

3.1.3 Experimental Results and Discussion 470

3.1.3.1 Comparison of Accuracy and

Precision for Fortification

Recovery Experiments by the

Three Methods 470

3.1.3.2 Correlation Comparison of the

Three Methods’ Extraction Efficiency

with Pesticide log Kow Values 471

3.1.3.3 General Analysis of Method Applicability 474

3.1.3.4 Comparison of the Cleanup Efficiency for the Three Methods 478

3.1.4 Conclusions 478

References 482

3.2 Uncertainty Evaluation of the

Determination of Multipesticide

Residues in Tea by Gas

Chromatography–Tandem Mass

Spectrometry Coupled with Three

Different Pretreatment Methods 483

3.2.1 Introduction 483

3.2.2 Reagents and Materials 484

3.2.3 Apparatus 485

3.2.4 Experimental Method 485

3.2.4.1 Method 1 (M1) 485

3.2.4.2 Method 2 (M2) 486

3.2.4.3 Method 3 (M3) 486

3.2.5 Estimation of Uncertainty 487

3.2.5.1 Identification of Uncertainty Sources 487

3.2.5.2 Calculation of Standard Uncertainty 489

3.2.6 Combined Uncertainty 497

3.2.7 Expanded Uncertainty 497

3.2.8 Result and Discussion 497

3.2.8.1 Uncertainty of M1 497

3.2.8.2 Uncertainty of M2 499

3.2.8.3 Uncertainty of M3 499

3.2.8.4 Comparison of the Three Methods for Uncertainty Analysis 500

3.2.9 Conclusion 503

References 504