茶叶农药多残留检测方法学研究(Analysis of Pesticide in Tea:Chromatography-Mass Spectrometry Methodology)
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书 名: 茶叶农药多残留检测方法学研究(Analysis of Pesticide in Tea:Chromatography-Mass Spectrometry Methodology) |
作 者: 庞国芳 著 |
I S B N: 34411 |
完整书号: 978-7-122-34411-3 |
出版年份: 2019 |
出版月份: 10 |
版 / 印次: 1-1 |
定 价: 888.00 |
开 本: 16 |
编辑推荐:
本书是与Elsevier合作出版项目,详细介绍了一系列测定茶叶中农药残留的快速高通量分析方法,具有高精度、高可靠性、高灵敏度的特点,适用广泛。作者庞国芳院士是农药及化学污染物残留分析领域的国际知名专家。
内容简介;
本书详细介绍了一系列测定茶叶中农药残留的快速高通量分析方法,具有高精度、高可靠性、高灵敏度的特点,适用广泛。全书共7章:茶叶农药残留分析基础研究和检测方法建立;不同样品制备技术提取净化效能对比研究;茶叶水化对农药多残留方法效率的影响;茶叶农药残留测定基质效应及其补偿作用研究;方法耐用性系统评价,误差原因分析,关键控制点建立;茶叶陈化样品和污染样品农药降解规律研究;经11个国家和地区30个实验室国际协同研究,建立茶叶中653种农药化学污染物高通量分析方法AOAC标准。
本书可作为科研单位、高等院校、质检机构等各类专业技术人员从事食品安全、环境保护、农业科技及农药开发等技术研究与应用的参考书,也可作为大学教学参考书。
作者简介:
庞国芳,中国检验检疫科学研究院,研究员,中国工程院院士,国家质检总局首席研究员、国际公职化学家联合会(AOAC)专家,国际AOAC 2014年度 Harvey W. Wiley 奖获得者。近30年一直工作在食品检验检疫一线,致力于食品科学检测技术理论与实践的研究,解决了我国相关出口食品、农产品等遭遇的技术瓶颈,为推动我国对外贸易发展做出了杰出贡献。研究制定了141项国际、国家检测技术标准。在国内、国际出版食品安全检测技术论著10部。发表论文100余篇,35篇被SCI收录。3次荣获国家科学技术进步二等奖,6次荣获国际AOAC组织颁发的科学技术奖励。
前言:
In China, tea has a long history. It is a unique Chinese health drink which is
popular with people all over the world. It is also an important cash crop and a
traditional bulk export agricultural product in China. As tea plants like to
grow in hot and humid environment, so their growth process is very susceptible
to diseases and insect pests and weeds, and chemical pesticide spraying is the
most effective solution so far. However, chemical pesticides leave undesirable
residues in tea in accompany with the increment of yield and these residues will
affect human health through the food chain. In addition, the developed countries
and regions, such as the European Union, the United States, and Japan, are
important importers of Chinese tea. The increasingly strict pesticide residue
limit standards (MRLs) have become an important bottleneck in China’s tea
export. Therefore, from the protection of human health, to eliminate trade
barriers, and to safeguard the perspective of international trade of tea, the
thorough study of the detection technique of multipesticide residues in tea and
the establishment of a highsensitivity, accuracy, selectivity, and throughput
detection method have extremely important practical significance.
This book
is the systematic summarization of the research of our team on the detection
technology theory and application of the multipesticide residues in tea products
in last 10 years. The book describes in detail the high-throughput analytical
techniques for 653 multiclasses and multikinds of pesticide residues and
chemical pollutants in tea, while the mainstream and advanced detection means
such as gas chromatography–mass spectrometry (GC–MS), gas chromatography–tandem
mass spectrometry (GC-MS/MS), liquid chromatography–tandem mass spectrometry
(LC–MS/MS), gas chromatography quadrupole tandem time-of-flight mass
spectrometry (GC-Q-TOF), and liquid chromatography quadrupole tandem timeof-
flight mass spectrometry (LC-Q-TOF) are concerned.
Compared with other
plant-derived agricultural products such as vegetables and fruits, the
composition of tea is extremely complex for it is rich in physiologically active
compounds such as polyphenols, alkaloids, pigments, aromatic substances, amino
acids, vitamins, and so on, and the composition varies greatly with processing
procedure, so it is considerable difficult for the detection of multiclasses and
multikinds of trace pesticide residues in tea.
Considering multiclasses and
multikinds of pesticides may exist in different tea matrix, deep research on the
comparison of the efficiency of various sample preparation technology and sample
purification technology is introduced in this book, and the Cleanert TPT tea
purification column, which has their own independent intellectual property
rights, was developed. The simultaneous extraction and purification pretreatment
method was established, while the matrix effect and its compensation of 28
different areas and species tea was deeply studied and the solution, using
protecting agent for the compensation of matrix effect, was put forward.
In
view of people’s drinking habits, the comparison of two extraction methods,
hydration method and nonhydration method, on the extraction efficiency,
purification effect of residual pesticides in tea, and the applicability of
different pesticides was conducted in-depth. At the same time, each component of
the uncertainty is discussed in detail, and the measurement uncertainty is
regarded as evaluation criteria of the method.
In addition, in order to
further evaluate the repeatability, reproducibility, and durability of the
method, the authors also carried out the evaluation of the ruggedness of the
method for up to 3 months. At the same time, concrete analysis has been made to
error types from different analytical stages and their causes, while elaborated
discussions have been conducted on the key control points in different stages of
the method to ensure the accurate and reliable of the method.
Furthermore,
the dynamics of pesticide degradation of aged oolong tea samples and
contaminated green tea samples at different field test and room temperature
storage conditions using the high-throughput detection method established were
carried by the author’s work team. The stability of the contaminated tea samples
within 3 months was also investigated, so as the degradation rule of pesticides
in tea can be obtained. So, the prediction of the content of pesticide residues
using degradation dynamic equation can be accomplished and the results are
basically consistent with the measured values. This has a very important
significance in offering guidance to tea growers to the applications of
pesticide and to the import and export trade of tea.
Based on the
aforementioned series of important research, the international collaborative
research, participated by a total of 30 laboratories from 11 countries and
regions, was organized and implemented by our team as the Study Director of AOAC
international and the purpose of the research is the evaluation of the
reproducibility of the analysis method for the 653 kinds of pesticide residues
in tea and investigation whether the method can meet the requirements of AOAC
international official method. This is overall comprehensive collaborative
research of AOAC international on the detection technical standards of pesticide
residue in tea, meanwhile the detailed report of the study is also included in
this book.
In short, a series of important studies about the detection
technology of multipesticide residues in tea are involved in this book and they
are the deepest and most comprehensive summary of high-throughput detection of
multipesticide residues in tea till now. The method, high-throughput detection
of 653 multiclasses and multikinds of pesticide residues and chemical pollutants
using GC–MS, GC–MS/MS, and LC–MS/MS, was selected as AOAC international priority
research projects in 2010, and the method passed the AOAC international
collaborative study and was approved as AOAC international official method for
the detection of pesticide residues in tea (AOAC Official Method 2014.09) in
2014. Nevertheless, due to the limitations of the level, there may be
unavoidable errors. We would kindly ask the users of this publication to provide
feedback to the authors so that subsequent editions may be improved upon.
Guo-Fang Pang
October 10, 2017
目录(节选):
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
4 Matrix Effect for Determination of Pesticide
Residues in Tea
4.1 Review 505
4.1.1 Current Situation of Matrix Effect
505
4.1.2 Cluster Analysis and Its Application in Chemical Analysis
509
4.2 Study on the Matrix Effects of Different
Tea Varieties from
Different
Producing Areas 510
4.2.1 Introduction 510
4.2.2 Experimental
Materials 510
4.2.3 Preparation of a Test Sample 511
4.2.4 Instrumental
Analysis Condition 512
4.2.5 Qualitative Analysis of the Sample and Data
Processing 513
4.2.6 Matrix Effect Evaluation of GC–MS 513
4.2.7
Evaluation of the Matrix Effect in Determination of GC–MS/MS 517
4.2.8
Evaluation of the Matrix Effect in Determination of LC–MS/MS 520
4.3
Compensation for the Matrix
Effects in the Gas Chromatography–
Mass
Spectrometry Analysis of 186
Pesticides in Tea Matrices Using
Analyte
Protectants 523
4.3.1 Introduction 523
4.3.2 Experiment and Material
523
4.3.3 Experimental Method 524
4.3.4 Effect of Different Analyte
Protectants on Solvent Standards 524
4.3.5 Effects of Different Analyte
Protectant Combinations on Tea 527
4.3.6 Effectiveness Evaluation of
Analyte
Protectant Compensation Matrix
Effect Method 530
4.4
Compensation for the Matrix
Effects in the Gas Chromatography–
Mass
Spectrometry Analysis of 205
Pesticides in Tea Matrices 533
4.4.1
Introduction 533
4.4.2 Experimental Materials 533
4.4.3 Experimental
Method 533
4.4.4 Effect of Different Analyte Protectants on Solvent Standards
534
4.4.5 Effects of Different Analyte Protectant Combinations on Tea
534
4.4.6 Effectiveness Evaluation of
Analyte Protectant
Compensation
Matrix Effect Method 537
References 541
5 The
Evaluation of the Ruggedness
of the Method, Error Analysis, and
the Key
Control Points of
the Method
5.1 Introduction 567
5.2 Experiment
568
5.2.1 Reagents and Materials 568
5.2.2 Apparatus 569
5.2.3
Preparing Pesticides-Aged Tea Samples
and the Evaluation of Uniformity
for
Preparation 569
5.2.4 Experimental Method 569
5.3 Evaluation of the
Ruggedness of the Method 570
5.3.1 Reproducibility Comparison
of the First
Determination
RSD of Parallel Samples from
Pesticide-Aged Youden
Pair
Samples with 18 Circulative
Determination Values 570
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 571
5.4 Error
Analysis and Key Control Points 573
5.4.1 Error Analysis of Sample
Pretreatment and Key Control Points 573
5.4.2 The Effects of Equipment
Status
on Test Results (Error Analysis)
and Critical Control Point
574
5.4.3 Chromatographic Resolution (Error Analysis)and Key Control Points
578
5.5 Conclusions 593
References 783
6 Study on the Degradation
of Pesticide Residues in Tea
6.1 Study on the Degradation of 271
Pesticide
Residues in Aged Oolong Tea
by Gas Chromatography-Tandem Mass
Spectrometry
and Its Application in
Predicting the Residue Concentrations of
Target
Pesticides 787
6.1.1 Introduction 787
6.1.2 Reagents and Material
788
6.1.2.1 Reagents 788
6.1.2.2 Material 788
6.1.3 Apparatus and
Conditions 788
6.1.4 Sample Pretreatment 789
6.1.4.1 The Preparation
Procedures for Aged Tea Samples 789
6.1.4.2 Extraction 789
6.1.4.3 Cleanup
789
6.1.5 The Degradation of 271 Pesticides in Aged Oolong Tea 789
6.1.5.1
Degradation Trend A 790
6.1.5.2 Degradation Trend B 791
6.1.5.3
Degradation Trend C 791
6.1.5.4 Degradation Trend D 792
6.1.5.5
Degradation Trend E 792
6.1.5.6 Degradation Trend F 792
6.1.6 Pesticides
in Different Classes 793
6.1.7 The Practical Application of Degradation
Regularity 794
6.1.7.1 The Degradation Regularity of 20 Representative
Pesticides 794
6.1.7.2 The Prediction of Pesticide Residues in Aged Oolong
Tea 795
6.1.8 Conclusions 797
References 799
6.2 A GC–MS, GC–MS/MS and
LC–MS/MS
Study of the Degradation Profiles of
Pesticide Residues in Green
Tea 801
6.2.1 Introduction 801
6.2.2 Reagents and Materials 802
6.2.3
Design of Field Trials 802
6.2.3.1 Selection of Pesticide Varieties
802
6.2.3.2 Selection and Planning of Tea Plantations 802
6.2.3.3
Pesticide Application and Incurred Tea Sample Preparations 803
6.2.4
Analytical method 804
6.2.4.1 Extraction and Cleanup 804
6.2.4.2 Apparatus
Conditions 804
6.2.5 The Pesticide Degradation Profiles within 30 days for
the Field Trials 805
6.2.6 Study on Pesticide Degradation by Three Techniques
805
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 807
6.2.8 Stability Study on the Pesticides in
Incurred
Tea Samples at Room Temperature Storage
Conditions (18–25°C)
809
6.2.9 Conclusions 810
6.2.10 Acknowledgments 810
References 810
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