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。
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
ChromatographyMass Spectrometry
GCMS and Liquid Chromatography
Tandem Mass Spectrometry
LCMSMS 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
ChromatographyMass Spectrometry
Conditions and Selection of Pesticide
Varieties Suitable for Analysis 6
1.1.3.2 Optimization of Liquid
ChromatographyTandem 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
ChromatographyMass Spectrometry
and Liquid ChromatographyTandem
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-TOFMS 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
內容試閱:
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 Chinas 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 chromatographymass spectrometry GCMS, gas chromatographytandem mass spectrometry GC-MSMS, liquid chromatographytandem mass spectrometry LCMSMS, 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 peoples 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 authors 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 GCMS, GCMSMS, and LCMSMS, 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