內容大鋼
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凈化效能對比研究；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應用的參考書，也可作為大學教學參考書。
目錄
Preface
Introduction
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)
1.1.1 Introduction
1.1.2 Experimental
1.1.2.1 Reagents and Materials
1.1.2.2 Apparatus
1.1.2.3 Extraction
1.1.2.4 Cleanup
1.1.2.5 Determination
1.1.3 Results and Discussion
1.1.3.1 Optimization of Gas
Chromatography–Mass SpectrometryConditions and Selection of PesticideVarieties Suitable for Analysis
1.1.3.2 Optimization of Liquid
Chromatography–Tandem Mass
Spectrometry Conditions and
Selection of Pesticide Varieties
Suitable for Analysis
1.1.3.3 Optimization of Sample Extraction
Conditions
1.1.3.4 Optimization of Sample Cleanup
Conditions
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
References
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
1.2.1 Introduction
1.2.2 Experimental
1.2.2.1 Reagents, Standard, and Materials
1.2.2.2 Equipment
1.2.2.3 Condition of Gas Chromatography and Mass Spectrometry
1.2.2.4 Pretreatment Methods for the Screening Analysis of Tea Samples
1.2.3 Establishment of Database
1.2.4 Evaluation of the Effi ciency of the Method
1.2.4.1 Qualitative Analysis
1.2.4.2 Screening Limit
1.2.4.3 Recovery (Rec. 60%–120%&RSD < 20%)
1.2.4.4 Comprehensive Analysis
(Comparative Analysis the Infl uence
of Matrix on the Screening Limit
and Recovery of Pesticides)
1.2.5 Conclusion
1.3 A Study of Effi ciency Evaluation for
Nontarget and High-Throughput
Screening of 556 Pesticides Residues
by LC-Q-TOF/MS
1.3.1 Introduction
1.3.2 Experimental
1.3.2.1 Reagents and Materials
1.3.2.2 HPLC Conditions
1.3.2.3 Mass Spectrometry Conditions
1.3.2.4 Sample Preparation
1.3.3 Creation of the Pesticide Database
1.3.4 Method Evaluation
1.3.4.1 Qualitative Analysis
1.3.4.2 Screening Limits
1.3.4.3 Accuracy and Precision
1.3.4.4 Comprehensive Analysis of Screening Limits and Recoveries
1.3.5 Conclusions
1.4 A Study of Effi ciency Evaluation for
Nontarget Screening of 1050 Pesticide
By TOFMS and
LC–Q–TOF/MS
1.4.1 Introduction
1.4.2 Experimental
1.4.2.1 Reagents and Materials
1.4.2.2 Standard Solution Preparation
1.4.2.3 Sample Collection and Pretreatment
1.4.2.4 Instrumental Analysis
1.4.2.5 Creation of the Pesticides Database
1.4.2.6 Method Evaluation
1.4.3 Results and Discussion
1.4.3.1 Screening Limits Analysis
1.4.3.2 Accuracy and Precision
1.4.3.3 Comparison of the Common-Detected Pesticides
1.4.4 Conclusion
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
2.1.1 Review of Solid Phase Extraction Technique
2.1.2 Review of QuEChERS Method
References
2.2 Comparative Study of Extraction
Effi ciencies of the Three Sample
Preparation Techniques
2.2.1 Introduction
2.2.2 Experimental
2.2.2.1 Reagents and Materials
2.2.2.2 Apparatus
2.2.2.3 Experimental Method
2.2.3 Preparing Pesticides Incurred Tea
Samples and Deciding the Precipitated
Content of the Target Pesticide
2.2.4 Optimization of Experimental Conditions for Method-
2.2.5 Optimization of the Evaporation
Temperatures and Degrees of the
Sample Solutions for Three Methods
2.2.5.1 Optimization Selection
of Temperatures of Rotary
Evaporation
2.2.5.2 Optimum Selection of the Degree of Rotary Evaporation
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-
2.2.6.1 Test Data Analysis
2.2.6.2 Analysis of Experimental Phenomenon
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-
2.2.8 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-
2.2.8.1 Test Data Analysis
2.2.8.2 Test Phenomenon Analysis
2.2.9 Conclusions
2.3 The Evaluation of the Cleanup
Effi ciency of SPE Cartridge Newly
Developed for Multiresidues
in Tea
2.3.1 Introduction
2.3.2 Reagents and Materials
2.3.3 Apparatus
2.3.4 Experimental
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
2.3.6 Stage II: The Comparative Test on
Cleanup Effi ciencies of Spiked
Pesticides in Tea with 4# Envi-Carb+PSA
Tandem Cartridge and Cleanert TPT
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
2.3.7.1 Comparison of the Determined
Values of Target Pesticide
Content
2.3.7.2 Comparison of the Reproducibility
of the Target Pesticide
Determination
2.3.8 Conclusions
References
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
3.1.1 Introduction
3.1.2 Experimental Method
3.1.2.1 Three Different Sample Preparation Methods
3.1.2.2 Aged Sample Preparation
3.1.2.3 Incurred Sample Preparation
3.1.3 Experimental Results and Discussion
3.1.3.1 Comparison of Accuracy and
Precision for Fortification
Recovery Experiments by the
Three Methods
3.1.3.2 Correlation Comparison of the
Three Methods』 Extraction Efficiency
with Pesticide log Kow Values
3.1.3.3 General Analysis of Method Applicability
3.1.3.4 Comparison of the Cleanup Efficiency for the Three Methods
3.1.4 Conclusions
References
3.2 Uncertainty Evaluation of the
Determination of Multipesticide
Residues in Tea by Gas
Chromatography–Tandem Mass
Spectrometry Coupled with Three
Different Pretreatment Methods
3.2.1 Introduction
3.2.2 Reagents and Materials
3.2.3 Apparatus
3.2.4 Experimental Method
3.2.4.1 Method 1 (M1)
3.2.4.2 Method 2 (M2)
3.2.4.3 Method 3 (M3)
3.2.5 Estimation of Uncertainty
3.2.5.1 Identification of Uncertainty Sources
3.2.5.2 Calculation of Standard Uncertainty
3.2.6 Combined Uncertainty
3.2.7 Expanded Uncertainty
3.2.8 Result and Discussion
3.2.8.1 Uncertainty of M
3.2.8.2 Uncertainty of M
3.2.8.3 Uncertainty of M
3.2.8.4 Comparison of the Three Methods for Uncertainty Analysis
3.2.9 Conclusion
References
4 Matrix Effect for Determination of Pesticide Residues in Tea
4.1 Review
4.1.1 Current Situation of Matrix Effect
4.1.2 Cluster Analysis and Its Application in Chemical Analysis
4.2 Study on the Matrix Effects of Different
Tea Varieties from Different
Producing Areas
4.2.1 Introduction
4.2.2 Experimental Materials
4.2.3 Preparation of a Test Sample
4.2.4 Instrumental Analysis Condition
4.2.5 Qualitative Analysis of the Sample and Data Processing
4.2.6 Matrix Effect Evaluation of GC–MS
4.2.7 Evaluation of the Matrix Effect in Determination of GC–MS/MS
4.2.8 Evaluation of the Matrix Effect in Determination of LC–MS/MS
4.3 Compensation for the Matrix
Effects in the Gas Chromatography–
Mass Spectrometry Analysis of
Pesticides in Tea Matrices Using
Analyte Protectants
4.3.1 Introduction
4.3.2 Experiment and Material
4.3.3 Experimental Method
4.3.4 Effect of Different Analyte Protectants on Solvent Standards
4.3.5 Effects of Different Analyte Protectant Combinations on Tea
4.3.6 Effectiveness Evaluation of Analyte
Protectant Compensation Matrix
Effect Method
4.4 Compensation for the Matrix
Effects in the Gas Chromatography–
Mass Spectrometry Analysis of
Pesticides in Tea Matrices
4.4.1 Introduction
4.4.2 Experimental Materials
4.4.3 Experimental Method
4.4.4 Effect of Different Analyte Protectants on Solvent Standards
4.4.5 Effects of Different Analyte Protectant Combinations on Tea
4.4.6 Effectiveness Evaluation of
Analyte Protectant Compensation
Matrix Effect Method
References
5 The Evaluation of the Ruggedness
of the Method, Error Analysis, and
the Key Control Points of
the Method
5.1 Introduction
5.2 Experiment
5.2.1 Reagents and Materials
5.2.2 Apparatus
5.2.3 Preparing Pesticides-Aged Tea Samples
and the Evaluation of Uniformity for
Preparation
5.2.4 Experimental Method
5.3 Evaluation of the Ruggedness of the Method
5.3.1 Reproducibility Comparison
of the First Determination
RSD of Parallel Samples from
Pesticide-Aged Youden Pair
Samples with 18 Circulative
Determination Values
5.3.2 Evaluation of the Ruggedness of the Method
Based on the RSD of the Youden Pair Ratios
from the 3-Month Circulative
Experiment
5.4 Error Analysis and Key Control Points
5.4.1 Error Analysis of Sample Pretreatment and Key Control Points
5.4.2 The Effects of Equipment Status
on Test Results (Error Analysis)
and Critical Control Point
5.4.3 Chromatographic Resolution (Error Analysis)and Key Control Points
5.5 Conclusions
References
6 Study on the Degradation of Pesticide Residues in Tea
6.1 Study on the Degradation of
Pesticide Residues in Aged Oolong Tea
by Gas Chromatography-Tandem Mass
Spectrometry and Its Application in
Predicting the Residue Concentrations of
Target Pesticides
6.1.1 Introduction
6.1.2 Reagents and Material
6.1.2.1 Reagents
6.1.2.2 Material
6.1.3 Apparatus and Conditions
6.1.4 Sample Pretreatment
6.1.4.1 The Preparation Procedures for Aged Tea Samples
6.1.4.2 Extraction
6.1.4.3 Cleanup
6.1.5 The Degradation of 271 Pesticides in Aged Oolong Tea
6.1.5.1 Degradation Trend A
6.1.5.2 Degradation Trend B
6.1.5.3 Degradation Trend C
6.1.5.4 Degradation Trend D
6.1.5.5 Degradation Trend E
6.1.5.6 Degradation Trend F
6.1.6 Pesticides in Different Classes
6.1.7 The Practical Application of Degradation Regularity
6.1.7.1 The Degradation Regularity of 20 Representative Pesticides
6.1.7.2 The Prediction of Pesticide Residues in Aged Oolong Tea
6.1.8 Conclusions
References
6.2 A GC–MS, GC–MS/MS and LC–MS/MS
Study of the Degradation Profiles of
Pesticide Residues in Green Tea
6.2.1 Introduction
6.2.2 Reagents and Materials
6.2.3 Design of Field Trials
6.2.3.1 Selection of Pesticide Varieties
6.2.3.2 Selection and Planning of Tea Plantations
6.2.3.3 Pesticide Application and Incurred Tea Sample Preparations
6.2.4 Analytical method
6.2.4.1 Extraction and Cleanup
6.2.4.2 Apparatus Conditions
6.2.5 The Pesticide Degradation Profiles within 30 days for the Field Trials
6.2.6 Study on Pesticide Degradation by Three Techniques
6.2.7 Comparison of the Pesticides Degradation
to MRL Actual Values in Field Trials with
Power Function Equations Predicted Values
Detected by Three Techniques
6.2.8 Stability Study on the Pesticides in Incurred
Tea Samples at Room Temperature Storage
Conditions (18–25°C)
6.2.9 Conclusions
6.2.10 Acknowledgments
References
7 High-Throughput Analytical
Techniques for Determination of
Residues of 653 Multiclass Pesticides
and Chemical Pollutants in Tea by
GC–MS, GC–MS/MS and LC–MS/MS:
Collaborative Study
7.1 The Pre-Collaborative Study of AOAC Method Efficiency Evaluation
7.1.1 Introduction
7.1.2 Design of Collaborative Study
7.1.2.1 Selection of Representative Pesticides
7.1.2.2 Preparation and Homogeneity Evaluation of Aged Samples
7.1.2.3 Types and Quantity of Collaborative Study Samples
7.1.2.4 Organizing and Implementing of Collaborative Study
7.1.2.5 System Suitability Check
7.1.2.6 Requirement for Participating in Collaborative Laboratories
7.1.3 Experiment
7.1.3.1 Instruments and Reagents
7.1.3.2 Preparation of Standard Solutions
7.1.3.3 Sample Preparation
7.1.3.4 Test Condition
7.1.4 Method Efficiency Acceptance Criteria
7.1.4.1 General Principle
7.1.4.2 Standard Curve Linear Correlation Coefficient Acceptance Criteria
7.1.4.3 Target Pesticide Ion Abundance Ratio Criteria
7.1.4.4 Recovery, RSDr, and RSDR Acceptance Criteria
7.1.4.5 Outliers Elimination Via Grubbs and Dixon Double Checking
7.1.5 Result and Discussion
7.1.5.1 The Labs That Deviated
from the Operational Method
Have Been Eliminated
7.1.5.2 Eliminations of Outliers Via
Double-Checking of Grubbs
and Dixon
7.1.5.3 Method Efficiency
7.1.5.4 Qualification and Quantification
7.1.5.5 Error Analysis and Tracing
7.1.6 Conclusions
References
7.2 Collaborative Study
7.2.1 Introduction
7.2.2 Collaborative Study Protocol
7.2.2.1 Need/Purpose
7.2.2.2 Scope/Applicability
7.2.2.3 Materials/Matrices
7.2.2.4 Concentrations/Ranges of Analytes
7.2.2.5 Spiked Samples of Blind Duplication
7.2.2.6 Naturally Incurred Residues Matrices
7.2.2.7 Sample Preparation and Handing Homogeneity
7.2.2.8 Quality Assurance
7.2.3 Method Performance Parameters for Single Laboratory
7.2.3.1 Limit of Detection and Limit of Quantification
7.2.3.2 Accuracy and Precision for a Single Laboratory
7.2.3.3 Linearity of 653 Pesticides for Single Laboratory
7.2.3.4 Ruggedness of Multiresidue Method
7.2.4 Collaborators
7.2.4.1 Instrument and Materials Used by Collaborators
7.2.5 AOAC Official Method: High-Throughput
Analytical Techniques for Determination of
Residues of 653 Multiclass Pesticides and
Chemical Pollutants in Tea by GC–MS, GC–
MS/MS, and LC–MS/MS
7.2.5.1 Principle
7.2.5.2 Apparatus and Conditions
7.2.5.3 Reagents and Materials
7.2.5.4 Preparation of Standard Solutions
7.2.5.5 Extraction and Cleanup Procedure
7.2.5.6 Qualitative and Quantitative
7.2.6 Results and Discussion
7.2.6.1 Evaluation of Collaborative Study Results
7.2.6.2 The Method Efficiency of the
Fortification Samples by GC–MS,
GC–MS/MS, and LC–MS/MS
7.2.6.3 The Method Efficiency of the Aged
Samples by GC–MS, GC–MS/MS,
and LC–MS/MS
7.2.6.4 The Method Efficiency of the
Incurred Samples by GC–MS,
GC–MS/MS, and LC–MS/MS
7.2.7 Qualification and Quantification
7.2.7.1 Qualification of Target Pesticides
7.2.7.2 Quantification of Target Pesticides
7.2.8 Error Analysis and Traceability
7.2.8.1 GC–MS Data Error Analysis and Traceability
7.2.8.2 GC–MS/MS Data Error Analysis and Traceability
7.2.8.3 LC–MS/MS Data Error Analysis and Traceability
7.2.9 Collaborators』 Comments on Method
7.2.9.1 Collaborators』 Comments on GC–MS
7.2.9.2 Collaborators』 Comments on GC–MS/MS
7.2.9.3 Collaborators』 Comments on LC–MS/MS
7.2.10 Conclusions
References
Index
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