Pesticide Analytical Manual Vol. I Regulatory Operations Chapter 2 General Analytical Operations and Information Chapter 3 Chapter 4 Multiclass Selective MRMS MRMS Chapter 5 GLC Chapter 6 HPLC Table of c page d 60l General Information 601 A: Principles 601-1 1/94 601 B: Modes of Operation 601-21/94 Liquid-Solid Chromatography 1/94 Liquid-Liquid Chromatography 601-31/94 Bonded Phase Chromatography 601-3 1/94 matograpl Size Exclusion Chromatography 601-41/94 601 C: Instrumentation and Apparatus 601-5 1/94 HPLC System Plumbing 60l-7 1/94 601 D: Solvents and Reagents 601-101/94 Potential Problems 601-101/94 Solve 601-121/94 Transmittal No. 96-E1 [9/96) Form FDA 2905a(6/92] 6Oo-1
Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92) 600–1 Pesticide Analytical Manual Vol. I SECTION 600 Table of Contents page date 601: General Information 601 A: Principles 601-1 1/94 601 B: Modes of Operation 601-2 1/94 Liquid-Solid Chromatography 601-2 1/94 Liquid-Liquid Chromatography 601-3 1/94 Bonded Phase Chromatography 601-3 1/94 Ion Exchange Chromatography 601-4 1/94 Size Exclusion Chromatography 601-4 1/94 601 C: Instrumentation and Apparatus 601-5 1/94 Basic Components 601-5 1/94 HPLC System Plumbing 601-7 1/94 601 D: Solvents and Reagents 601-10 1/94 Potential Problems 601-10 1/94 Specific Solvents 601-12 1/94 Chapter 1 Regulatory Operations Chapter 2 General Analytical Operations and Information Chapter 3 Multiclass MRMs Chapter 5 GLC Chapter 4 Selective MRMs Chapter 6 HPLC
Pesticide Analytical Manual Vol I Reagent blanks 601-141/94 1-141/94 601 E: Sample preparation 601-141/94 601-141/94 Sample filtration 601-141/94 601-151/94 Choice of Sample solvent 601-151/94 601-151 Stock solutions 601-151/94 dard soluti 601-161/9 01-161/94 Refe 601-161/9 602 Columns 02 A Column selection 602-11/94 602 B: Analytical Columns 602-1 Liquid-Solid Chromatography 60221/94 Bonded phases 6022 1/94 Ion exchange 60231/94 Ion pair 6024 1/94 Size exclusion 602 C: Column evaluation 602-5 1/94 602 D: Column Specifications 60261/94 602 E: Analytical Column Protection 60281/94 Filters 60281/94 Precolumns 60291/94 Guard columns 60291/94 602 F: Column Maintenance and Troubleshooting 602-9 1/94 Column Care 602-9 Column Evaluation by Injection of 602-101/94 Test mixtures Column Storage 602-111/94 Column Regeneration 602-111/94 References 602-121/94 603: Mobile Phase Selection, Preparation, and Delivery 603 A: Mobile phase Selection 60311/9 Normal Phase Chromatography 60311/94 R aphy 60331/94 lon Exchange Chromatography 60341/94 Ion Pair Chromatography 60351/94 Size Exclusion Chromatography 60351/94 Gradient Elution in HPlc 60351/94 603 B: Mobile Phase Preparation 60361/94 Filtering Solvents 60361/94 Degassing solvents 6036 1/94 600-2 Transmittal No.9七19/96 Form FDA 2905a(6/92]
Transmittal No. 96-E1 (9/96) 600–2 Form FDA 2905a (6/92) SECTION 600 Pesticide Analytical Manual Vol. I page date Reagent Blanks 601-14 1/94 Safety Precautions 601-14 1/94 601 E: Sample Preparation 601-14 1/94 Sample Cleanup 601-14 1/94 Sample Filtration 601-14 1/94 Sample Solvent Degassing 601-15 1/94 Choice of Sample Solvent 601-15 1/94 601 F: Reference Standards 601-15 1/94 Stock Solutions 601-15 1/94 Working Standard Solutions 601-16 1/94 Storage 601-16 1/94 References 601-16 1/94 602: Columns 602 A: Column Selection 602-1 1/94 602 B: Analytical Columns 602-1 1/94 Liquid-Solid Chromatography 602-2 1/94 Bonded Phases 602-2 1/94 Ion Exchange 602-3 1/94 Ion Pair 602-4 1/94 Size Exclusion 602-4 1/94 602 C: Column Evaluation 602-5 1/94 602 D: Column Specifications 602-6 1/94 602 E: Analytical Column Protection 602-8 1/94 Filters 602-8 1/94 Precolumns 602-9 1/94 Guard Columns 602-9 1/94 602 F: Column Maintenance and Troubleshooting 602-9 1/94 Column Care 602-9 1/94 Column Evaluation by Injection of 602-10 1/94 Test Mixtures Column Storage 602-11 1/94 Column Regeneration 602-11 1/94 References 602-12 1/94 603: Mobile Phase Selection, Preparation, and Delivery 603 A: Mobile Phase Selection 603-1 1/94 Normal Phase Chromatography 603-1 1/94 Reverse Phase Chromatography 603-3 1/94 Ion Exchange Chromatography 603-4 1/94 Ion Pair Chromatography 603-5 1/94 Size Exclusion Chromatography 603-5 1/94 Gradient Elution in HPLC 603-5 1/94 603 B: Mobile Phase Preparation 603-6 1/94 Filtering Solvents 603-6 1/94 Degassing Solvents 603-6 1/94
Pesticide Analytical Manual Vol. I Preparation of Multisolvent Mobile Phases 603-7 1/94 Solvent reservoir 603-71/94 603 C: Mobile Phase delivery systems 60381/94 603-8 Gradient Programming Systems 603-101/94 603 D: Maintenance and Troubleshooting 603-101/94 Problems with Pumps 603-101/94 603-131/94 604 Ir 604 A: Injection Valves 604-1 1/94 604 B: Automatic Injectors 604-31/ 604 C: Operation, Maintenance, Troubleshooting, 604-3 and Repair of Inje References 604-41/94 605 A: UV/VIS Absorbance Detectors 1/94 Fixed Wavelength UV Detectors Variable wavelength uv detectors 6054 1/94 Solvents 60541/94 Performance characteristic 60541/94 Multichannel or Photodiode array Detectors 605-5 1/94 Ap Problems, Maintenance and 605-5 1/94 605 B: Fluorescence detectors 605-6 1/94 Detector design 605-61/94 605-71 Performance characteristics 605-7 1/94 Parameter Adjustments 605-8 605-8 1/94 Detector maintenance 605-8 1/94 605 C: Electrochemical detectors 60581/94 Conductivity Detectors 605-91/94 mperometric and Coulometric Detectors 605-9 1 Performance characteristics 605-101 605 D: Photoconductivity Detectors 605-111/94 Apparatus 605-111/94 Performance Characteristics 605-111/94 cations 605-131/94 605 E: Mass Spectrometric Detectors 605-131/94 605 F: Derivatization for detection enhancement 605-141/94 Comparison of Pre- and Post-Column 605-141/94 Derivatizati Transmittal No. 96-E1 [9/96) Form FDA 2905a(6/92] 6O0-3
Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92) 600–3 Pesticide Analytical Manual Vol. I SECTION 600 page date Preparation of Multisolvent Mobile Phases 603-7 1/94 Solvent Reservoirs 603-7 1/94 603 C: Mobile Phase Delivery Systems 603-8 1/94 Pumps 603-8 1/94 Gradient Programming Systems 603-10 1/94 603 D: Maintenance and Troubleshooting 603-10 1/94 Problems with Pumps 603-10 1/94 References 603-13 1/94 604: Injection Systems 604 A: Injection Valves 604-1 1/94 604 B: Automatic Injectors 604-3 1/94 604 C: Operation, Maintenance, Troubleshooting, 604-3 1/94 and Repair of Injection Valves References 604-4 1/94 605: Detectors 605 A: UV/VIS Absorbance Detectors 605-2 1/94 Fixed Wavelength UV Detectors 605-3 1/94 Variable Wavelength UV Detectors 605-4 1/94 Solvents 605-4 1/94 Performance Characteristics 605-4 1/94 Multichannel or Photodiode Array Detectors 605-5 1/94 Applications 605-5 1/94 Problems, Maintenance, and 605-5 1/94 Troubleshooting 605 B: Fluorescence Detectors 605-6 1/94 Detector Design 605-6 1/94 Solvents 605-7 1/94 Performance Characteristics 605-7 1/94 Parameter Adjustments 605-8 1/94 Applications 605-8 1/94 Detector Maintenance 605-8 1/94 605 C: Electrochemical Detectors 605-8 1/94 Conductivity Detectors 605-9 1/94 Amperometric and Coulometric Detectors 605-9 1/94 Performance Characteristics 605-10 1/94 Applications 605-11 1/94 605 D: Photoconductivity Detectors 605-11 1/94 Apparatus 605-11 1/94 Performance Characteristics 605-11 1/94 Applications 605-13 1/94 605 E: Mass Spectrometric Detectors 605-13 1/94 605 F: Derivatization for Detection Enhancement 605-14 1/94 Comparison of Pre- and Post-Column 605-14 1/94 Derivatization
Pesticide Analytical Manual Vol I Post-Column Reactor design 605-141/94 References 605-161/94 606: Residue Identification and Quantitation 606A: Residue identification 606-11/9 Co-chromatography 6061 1/94 Use of Alternative columns 60621/94 Spectrometric Confirmation 60621/9 606 B: Quantitation 60631/94 Reference 606-31/9 7: Quality Assurance and Troubleshooting 607 A: Liquid Chromatograph Monitoring and 607-11/94 Performance Testing 607B: Troubleshooting from Chromatograms 607-21/94 Bibliography General Texts 60811/94 Columns 608-1 1/94 Detectors 60821/94 Troubleshooting 608-2 1/94 Application to Pesticides 6082 Fi 601-a Chromatographic Separation Techniques 601-11/94 601-b HPLC Modes of Operation 601-2 1/94 601-c Guide to Selection of HPLC Mode 601-5 601-d Block Diagram of HPLC System 1/94 601 Column Outlet Fitting 60171/94 601-f Low Dead Volume Fitting 601-71/94 601-g Standard Internal Fittin 601-81/94 60l-h Internal Thread Low dead Volume fitting 6018 602-a Calculation of Column Performance Parameters 602-5 1/94 603-a Reciprocating Pump 60381/94 603-b Gradient System I 60391/94 603-c Gradient System II 60391/94 603-d Gradient System Ill 603101/94 604-a External Loop Injector: Six-Port Injection Valve 604-1 1/94 Fb Internal Loop Injector 605-a UV/VIS Detector 605-b Variable Wavelength UV/VIS Detector 60541/94 605-c Fluorescence HPLC Detector 605-69/96 605-d Three electrode electrochemical detector 605-101/94 605-e Post-Column reactors 605-151/94 Transmittal No.9七19/96 Form FDA 2905a(6/92]
Transmittal No. 96-E1 (9/96) 600–4 Form FDA 2905a (6/92) SECTION 600 Pesticide Analytical Manual Vol. I page date Post-Column Reactor Design 605-14 1/94 References 605-16 1/94 606: Residue Identification and Quantitation 606 A: Residue identification 606-1 1/94 Co-chromatography 606-1 1/94 Use of Alternative Columns 606-2 1/94 Spectrometric Confirmation 606-2 1/94 606 B: Quantitation 606-3 1/94 Reference 606-3 1/94 607: Quality Assurance and Troubleshooting 607 A: Liquid Chromatograph Monitoring and 607-1 1/94 Performance Testing 607 B: Troubleshooting from Chromatograms 607-2 1/94 608: Bibliography General Texts 608-1 1/94 Columns 608-1 1/94 Detectors 608-2 1/94 Troubleshooting 608-2 1/94 Application to Pesticides 608-2 1/94 Figures 601-a Chromatographic Separation Techniques 601-1 1/94 601-b HPLC Modes of Operation 601-2 1/94 601-c Guide to Selection of HPLC Mode 601-5 1/94 601-d Block Diagram of HPLC System 601-6 1/94 601-e Column Outlet Fittings 601-7 1/94 601-f Low Dead Volume Fitting 601-7 1/94 601-g Standard Internal Fitting 601-8 1/94 601-h Internal Thread Low Dead Volume Fitting 601-8 1/94 602-a Calculation of Column Performance Parameters 602-5 1/94 603-a Reciprocating Pump 603-8 1/94 603-b Gradient System I 603-9 1/94 603-c Gradient System II 603-9 1/94 603-d Gradient System III 603-10 1/94 604-a External Loop Injector: Six-Port Injection Valve 604-1 1/94 604-b Internal Loop Injector 604-2 1/94 605-a UV/VIS Detector 605-3 1/94 605-b Variable Wavelength UV/VIS Detector 605-4 1/94 605-c Fluorescence HPLC Detector 605-6 9/96 605-d Three Electrode Electrochemical Detector 605-10 1/94 605-e Post-Column Reactors 605-15 1/94
Pesticide Analytical Manual Vol. I Tables 602-a: HPLC Column Specification Elements 602-71/94 602-b: Minimum Efficiency values 6028 603-a: Properties of Common HPLC Solvents with 603-2 1/94 Alu Columns 603-b: Classification of Solvent Selectivity 603-2 1/94 Transmittal No. 96-E1 [9/96) Form FDA 2905a(6/92] 6o05
Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92) 600–5 Pesticide Analytical Manual Vol. I SECTION 600 page date Tables 602-a: HPLC Column Specification Elements 602-7 1/94 602-b: Minimum Efficiency Values 602-8 1/94 603-a: Properties of Common HPLC Solvents with 603-2 1/94 Alumina Columns 603-b: Classification of Solvent Selectivity 603-2 1/94