Practical Approaches to Method Validation and Essential Instrument Qualification Book

Contributors

Preface

1 Overview of Risk-Based Approach to Phase Appropriate Validation and Instrument Qualification Wolfgang Winter Winter, Wolfgang 1

1 Risk-Based Approach to Pharmaceutical Development 1

2 Regulatory Requirements for Performance Verification of Instruments 3

3 General Approach to Instrument Performance Qualification 4

References 10

2 Phase Appropriate Method Validation Pramod Saraswat Saraswat, Pramod 11

1 Introduction 11

2 Parameters for Qualification and Validation 14

3 Qualification and Validation Practices 15

4 Common Problems and Solutions 25

References 25

3 Analytical Method Verification, Method Revalidation, and Method Transfer Pramod Saraswat Saraswat, Pramod 27

1 Introduction 27

2 Cycle of Analytical Methods 28

3 Method Verification Practices 28

4 Method Revalidation 36

5 Method Transfer 40

6 Common Problems and Solutions 42

References 43

4 Validation of Process Analytical Technology Applications Alison C. E. Harrington Harrington, Alison C. E. 45

1 Introduction 45

2 Parameters for Qualification and Validation 48

3 Qualification, Validation, and Verification Practices 56

4 Common Problems and Solutions 69

References 73

5 Validation of Near-Infrared Systems for Raw Material Identification Lenny Dass Dass, Lenny 75

1 Introduction 75

2 Validation of an NIR System 77

3 Validation Plan 78

References 90

6 Cleaning Validation Anthony Qu Qu, Anthony 93

1 Introduction 93

2 Scope of the Chapter 94

3 Strategies and Validation Parameters 94

4 Analytical Methods in Cleaning Validation 100

5 Sampling Techniques 102

6 Acceptance Criteria of Limits 104

7 Campaign Cleaning Validation 107

8 Common Problems and Solutions 108

References 110

7 Risk-Based Validation of Laboratory Information Management Systems R. D. McDowall McDowall, R. D. 111

1 Introduction 111

2 LIMS and the LIMS Environment 114

3 Understanding and Simplifying Laboratory Processes 117

4 GAMP Software Categories and System Life Cycle for a LIMS 121

5 Validation Roles and Responsibilities for a LIMS Project 124

6 System Life-Cycle Detail and Documented Evidence 126

7 Maintaining the Validated Status 147

8 Summary 151

References 152

8 Performance Qualification and Verification of Balance Ian Ciesniewski Ciesniewski, Ian 155

1 Introduction 155

2 Performance Qualification 159

3 Common Problems and Solutions 161

References 169

Appendix 170

9 Performance Verification of NIR Spectrophotometers Shauna Rotman Rotman, Shauna 177

1 Introduction 177

2 Performance Attributes 179

3 Practical Tips in NIR Performance Verification 192

References 195

Appendix 1 197

Appendix 2 199

10 Operational Qualification in Practice for Gas Chromatography Instruments Herman Lam Lam, Herman 201

1 Introduction 201

2 Parameters for Qualification 202

3 Operational Qualification 208

4 Preventive Maintenance 219

5 Common Problems and Solutions 220

References 229

11 Performance Verification on Refractive Index, Fluorescence, and Evaporative Light-Scattering Detection Richard W. Andrews Andrews, Richard W. 231

1 Introduction 231

2 Qualification of Differential Refractive Index Detectors 238

3 Qualification of Fluorescence Detectors 242

4 Qualification of Evaporative Light-Scattering Detectors 250

Reference 253

12 Instrument Qualification and Performance Verification for Particle Size Instruments Alan F. Rawle Rawle, Alan F. 255

1 Introduction 255

2 Setting the Scene 257

3 Particle Counting Techniques 258

4 Particle Size Analysis and Distribution 259

5 Instrument Qualification for Particle Size 260

6 Qualification of Instruments Used in Particle Sizing 272

7 Method Development 279

8 Verification: Particle Size Distribution Checklist 291

9 Common Problems and Solutions 292

10 Conclusions 295

References 295

Appendix 297

13 Method Validation, Qualification, and Performance Verification for Total Organic Carbon Analyzers Jose E. Martinez-Rosa Martinez-Rosa, Jose E. 299

1 Introduction 299

2 TOC Methodologies 302

3 Parameters for Method Validation, Qualification, and Verification 307

4 Qualification, Validation, and Verification Practices 310

5 Common Problems and Solutions 321

References 323

14 Instrument Performance Verification: Micropipettes Richard Curtis Curtis, Richard 327

1 Introduction 327

2 Scope of the Chapter 328

3 Verification Practices: Volume Settings, Number of Replicates, and Tips 338

4 Parameters: Accuracy, Precision, and Uncertainty 342

5 Summary 345

References 346

15 Instrument Qualification and Performance Verification for Automated Liquid-Handling Systems Keith J. Albert Albert, Keith J. 347

1 Introduction 347

2 Commonalities Between Volume Verification Methods for Performance Evaluation 354

3 Volume Verification Methods 356

4 Importance of Standardization 371

5 Summary 372

References 373

16 Performance Qualification and Verification in Powder X-Ray Diffraction Aniceta Skowron Skowron, Aniceta 377

1 Introduction 377

2 Basics of X-Ray Diffraction 378

3 Performance Qualification 381

4 Performance Verification: Calibration Practice 387

References 389

Index 391