Quality control of pesticide products

Format:

Book

Author/Creator:

International Atomic Energy Agency, Corporate Author.

Language:

English

Subjects (All):

Pesticides.

Analytical chemistry.

Physical Description:

1 online resource (241 pages)

Edition:

1st ed.

Place of Publication:

[Place of publication not identified] International Atomic Energy Agency 2009

Language Note:

English

Summary:

In light of an established need for more efficient analytical procedures, this publication, which documents the findings of an IAEA coordinated research project (CRP) on "Quality Control of Pesticide Products", simplifies the existing protocol for pesticide analysis while simultaneously upholding existing standards of quality. This publication includes both a report on the development work done in the CRP and a training manual for use by pesticide analysis laboratories. Based on peer reviewed and internationally recognized methods published by the Association of Analytical Communities (AOAC) and the Collaborative International Pesticides Analytical Council (CIPAC), this report provides laboratories with versatile tools to enhance the analysis of pesticide chemicals and to extend the scope of available analytical repertoires. Adoption of the proposed analytical methodologies promises to reduce laboratories' use of solvents and the time spent on reconfiguration and set-up of analytical equipment.

Contents:

Cover

FOREWORD

CONTENTS

SUMMARY

REFERENCES

GENERAL GUIDANCE

PRINCIPLES OF SINGLE-LABORATORY VALIDATION OF ANALYTICAL METHODS FOR TESTING THE CHEMICAL COMPOSITION OF PESTICIDES

1. INTRODUCTION

2. GENERAL PRINCIPLES

3. PERFORMANCE CHARACTERISTICS OF METHODS TO BE ESTABLISHED

3.1 Terms not used by CIPAC Guidelines but generally required for method validation

4. APPLICABILITY OF VALIDATION DATA TO MORE THAN ONE FORMULATION(ACCORDING TO THE CIPAC GUIDELINES)

5. VERIFICATION OF THE PERFORMANCE OF THE METHOD

5.1. Quality control of samples analyzed at irregular intervals

6. ADAPTATION OF A VALIDATED METHOD IN ANOTHER LABORATORY

6.1. The method is performed without any change

6.2. The method needs to be modified

APPENDIX I

APPENDIX II

APPENDIX III

STEPWISE PROCEDURE FOR DEVELOPMENT AND VALIDATION OF A MULTIPESTICIDE METHOD

1. PRINCIPLE OF MULTI-PESTICIDE METHODS

2. PRELIMINARY ACTIONS

3. SELECTION OF CHROMATOGRAPHIC SEPARATION AND DETECTION CONDITIONS AND VERIFICATION OF THEIR PERFORMANCE

3.1. Gas chromatographic determination

3.2. HPLC determination

3.3. Extension of the method for other pesticides

4. DETERMINATION OF THE LONG TERM REPEATABILITY AND REPRODUCIBILITY OF THE MULTI-PESTICIDE PROCEDURE

5. DOCUMENTATION OF LABORATORY WORK

PRINCIPLES OF DEVELOPING MULTI-PESTICIDE METHODS BASED ON GC DETERMINATION

1. SUMMARY

PRINCIPLES OF DEVELOPING MULTI-PESTICIDE METHODS BASED ON HPLC DETERMINATION

2. BASIC CONSIDERATIONS FOR HPLC METHOD DEVELOPMENT

2.1. Selection of chromatographic column

2.2. Selection of mobile phase

2.3. Column temperature

2.4. Flow rate

2.5. Injection volume and solvent

3. INTERNAL VERSUS EXTERNAL STANDARD METHOD

4. SYSTEM SUITABILITY TEST.

4.1. Performance of SST

THE UNCERTAINTY OF MEASUREMENT RESULTS

1. FACTORS AFFECTING THE PRECISION (UNCERTAINTY) OF THE MEASUREMENT RESULTS

1.1. Basic relationships of uncertainty components

2. ESTIMATION OF THE UNCERTAINTY OF THE MEASUREMENT RESULTS

2.1. Estimation of the repeatability and within-laboratory reproducibility of the results

2.2. Estimation of the uncertainty of individual steps of the method

3. PREPARATION OF SOLUTIONS WITH PRECISE CONCENTRATION OF ANALYTES

EXPERIMENTAL RESULTS

SUMMARY OF VALIDATION OF MULTI-PESTICIDE METHODS FOR VARIOUS PESTICIDE FORMULATIONS

2. WORKED-OUT EXAMPLE FOR THE VALIDATION OF A MULTI-PESTICIDE METHOD

2.1. Gas chromatographic conditions for lambda cyhalothrin

2.2. Sample preparation

2.3. Comparison of results obtained on two columns

3. SUMMARY OF REPEATABILITY OF GC INJECTIONS

4. ANALYSIS OF PESTICIDE FORMULATIONS

MULTI-PESTICIDE METHODS

GC 'MULTI-ANALYTE' DETECTION METHOD

2. STEPS OF METHOD DEVELOPMENT

3. CHROMATOGRAPHIC PROCEDURE

3.1 Apparatus and operating conditions

4. DETERMINATION OF RELATIVE RETENTION TIMES

4.1. Control of system suitability

REFERENCE

QUALITY CONTROL OF SELECTED PESTICIDES WITH GC1

MATERIALS AND METHODS

2.1. Materials

2.2. Sample Preparation

2.3. Gas chromatographic system and analysis conditions

2. VALIDATION OF THE MP METHOD

3.1. Performance characteristics of GC determination

3.2. Testing the specificity of the method

3.3. Batch Analysis

3.4. Method performance during routine analysis

APPLICATION OF MULTI-ANALYTE METHODS FOR PESTICIDE FORMULATIONS

2. MATERIALS AND METHODS

2.1. Conditions of GC analysis

2.2. Reagents.

2.3. Preparation of samples and standard solutions

2.4. Gas chromatographic analysis

3. RESULTS

3.1. Evaluation of results

HPLC 'MULTI-ANALYTE' DETECTION METHOD

3.2 Reagents

3.3 Recommended liquid chromatographic conditions for scouting run

4. DETERMINATION OF RELATIVE RETENTION TIMES FROM LINEAR GRADIENT RUN

4.1 Determination of the isocratic conditions

4.2. Spectral Analysis

QUALITY CONTROL OF SELECTED PESTICIDES WITH HPLC

2.1. HPLC system

2.2. Use of Chromolith RP-18e column

2.3. Use of Purosphere STAR RP-18 column

2.4. Analysis of different batches of commercial products

3. COMPARISON OF THE RESULTS OBTAINED ON TWO COLUMNS

MULTI-ANALYTE SEPARATION METHODS FOR HPLC DETERMINATION OF THE ACTIVE INGREDIENTS OF PESTICIDES

2.2. Reagents

2.3. Method

3. EVALUATION OF RESULTS

3.1. Characterization of chromatographic separation of several active ingredients

3.2. Comparison of the gradient programme to Dudar's programme

3.3. Elution sequence of pesticides based on their partition coefficient between n-octanol and water

3.4. Selection of wavelength and AUFS

3.5. Applicability of the separation system

SEPARATION AND SIMULTANEOUS DETERMINATION OF 14 FUNGICIDES WITH THE COMBINATION OF MULTI-ANALYTE METHODS AND HPLC DETECTION

2. EQUIPMENT AND MATERIALS

2.1. HPLC/MS system

2.2. Materials

SYNTHESIS AND DETERMINATION OF IMPURITIES

SYNTHESIS AND IDENTIFICATION OF SELECTED IMPURITIES

2. SYNTHESIS AND STRUCTURAL IDENTIFICATION OF IMPURITIES.

2.1. 2-ethyl-6-methyl-N-chloroacetanilide

2. 2. 2-ethyl-6-methyl-N-(methoxy-methyl)-chloroacetanilide

2.3. 2-ethyl-6-methyl-N- (ethoxy-methyl)-dichloroacetanilide

2.4. 2,4-dichloroisopropoxybenzene

2.5. Trimethylacetamide

2.6. 2-bromomethyl-2-(2,4-dichlorophenyl-4-propyl-1,3-dioxolan

2.7. 2,6-dimethylaniline

2.8. 3,5,6-trichloropyridin-2-ol

2.9. 3-nitrophenol (C6H4(NO2)OH)

2.10. 3-methyl-4-nitrophenol

2.11. 5-methyl-2-nitrophenol

2.12. O,O,O-trimethyl phosphorothioate ((CH3O)3PS)

2.13. O,O,O-triethyl phosphorothioate ((C2H5O)3PS)

2.14. Butyl 2-chloroacetate

2.15. 1,5-dichloro-2-(trifluoromethyl)-4-nitrobenzene (C6H2(NO2)(CF3)Cl2)

2.16. 2-chloro-5-(trifluoromethyl)-1,3-dinitrobenzene (C6H2(NO2)2(CF3)Cl)

3. IDENTIFICATION OF THE COMPOUNDS

3.1. Identification of impurities by infra red spectroscopy

3.2 Identification of Impurities by NMR

3.3. GC/MS spectra of compounds

4. GC ANALYSIS OF SYNTHESIZED COMPOUNDS

DETERMINATION OF IMPURITIES OF ATRAZINE BY HPLC-MS

2.2. GC/MS system

2.3. GC conditions for analysis of technical product

2.4. Chemicals

3. HPLC AND GC ANALYSIS OF IMPURITIES

4. SYNTHESIS AND IDENTIFICATION OF IMPURITIES

5. QUANTITATIVE ANALYSIS ON THE IMPURITIES OF TECHNICAL ATRAZINE

5.1. Preparation of standard and sample solutions

ANNEXES

Annex 1 UV spectra of compounds included in Section "HPLC 'MULTI-ANALYTE'DETECTION METHOD".

Annex 2 IR spectra of impurities synthesized

Annex 3 NMR spectra of impurities synthesized

Annex 4 GC/MS chromatograms and spectra of impurities synthesized

LIST OF ABBREVIATIONS

LIST OF PARTICIPANTS.

Notes:

Bibliographic Level Mode of Issuance: Monograph

Description based on publisher supplied metadata and other sources.

Part of the metadata in this record was created by AI, based on the text of the resource.

ISBN:

1-282-77523-5

9786612775239

OCLC:

794378008