Method Validation in Pharmaceutical Analysis -

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Résumé :

Preface xvii

1 Analytical Validation Within the Pharmaceutical Lifecycle 1
Phil Nethercote and Joachim Ermer

1.1 Development of Process and Analytical Validation Concepts 1

1.2 Alignments Between Process and Analytics: Three-Stage Approach 3

1.3 Predefined Objectives: ATP 5

1.4 Analytical Lifecycle 7

References 9

Part I Prerequisites 13

2 Data Governance, Data Integrity, and Data Quality 15
R.D. McDowall and C. Burgess

2.1 Terminology Used in This Chapter 15

2.2 Data Governance and Data Integrity Model 16

2.3 Interaction Between Levels 1 and 2 21

2.4 Overview of Data Integrity 21

2.5 ALCOA Criteria for Data Integrity 22

2.6 Understanding Level 3: Right Analysis for the Right Reportable Result 23

2.7 Second-Person Review 28

2.8 Summary 30

References 30

3 Analytical Instrument Qualification and System Validation Lifecycle 35
C. Burgess and R.D. McDowall

3.1 Data Integrity and Data Quality in a GMP Environment 35

3.2 AIQSV Approach as an Essential Part of the Analytical Procedure Lifecycle 37

3.3 USP General Chapter <1058> 38

3.4 Enhancement of <1058> and Harmonization of a Risk-Based Approach to Instruments and Systems with GAMP 43

3.5 Risk-Based Approaches to Analytical Instrument and System Qualification [3] 45

References 49

4 Continued HPLC Performance Qualification 51
Hermann W?tzig and Neil J. Lander

4.1 Introduction 51

4.2 Development of the Revised OQ/PQ Parameters List 53

4.3 Transfer of Modular Parameters into the Holistic Approach 55

4.4 OQ/PQ Data in Comparison with SST Data 58

4.5 Performance Monitoring: Trending Plots/Control Charts 59

4.6 General Procedure for cPQ 61

4.7 Example 65

4.8 Concluding Remarks 66

Acknowledgment 67

References 67

Part II Establishment of Measurement Requirements 69

5 Analytical Target Profile 71
Brent Harrington

5.1 Introduction 71

5.2 Components of an ATP 72

5.3 The Probability Statements 73

5.4 Metrics for Assessment 74

5.5 Summary 76

Acknowledgments 77

References 77

6 Decision Rules and Fitness for Intended Purpose 79
Jane Weitzel

6.1 Introduction 79

6.2 Defining the Fitness for Intended Purpose 80

6.3 Decision Rules 81

6.4 Overview of Process to Develop Requirements for Procedure Performance 82

6.5 Decision Rules and Compliance 82

6.6 Calculating Target Measurement Uncertainty 83

6.7 Types of Decision Rules 86

6.8 Target Measurement Uncertainty in the ATP 88

6.9 Bias and Uncertainty in a Procedure 89

6.10 ATP and Key Performance Indicators 89

6.11 Measurement Uncertainty 90

6.12 Example 94

6.13 Conclusion 95

References 96

7 Performance Characteristics of Analytical Procedures 97
Joachim Ermer

7.1 Precision 98

7.2 Accuracy 147

7.3 Specificity/Selectivity 167

7.4 Response (Calibration Model) 175

7.5 Detection and Quantitation Limits 193

Acknowledgments 205

References 206

Part III Method Design and Understanding 217

8 ICHQ14 Analytical Procedure Development 219
Phil Borman (GSK), Peter Hamilton (AZ), and Jean-Fran?ois Dierick (GSK)

8.1 Introduction 219

8.2 The ATP 220

8.3 Connection Between Product and Analytical Procedure Understanding 222

8.4 Prior and Platform Knowledge 223

8.5 Robustness and Method Operable ...

Biographie:

Joachim Ermer worked for 30 years in the pharmaceutical industry, including analytical development, global responsibilities, Head of Quality Control, and head of QC Lifecycle Management, before he started in December 2020 his consultancy business.

Phil W. Nethercote was the analytical leader for the Global Manufacturing and Supply Division of GSK until he retired in 2016. He has over 30 years of experience in the pharmaceutical industry, the majority of which has been with Glaxo, Glaxo Wellcome and GSK....

Sommaire:

New edition of the gold standard in the field of pharmaceutical analysis, extensively updated to include the new ICH Guidelines Q2(R2) and Q14

Following a holistic lifecycle approach to analytical procedures, Method Validation in Pharmaceutical Analysis provides hands-on information for readers involved in development, validation, and continued maintenance and evaluation of analytical procedures in pharmaceutical analysis.

This newly revised and updated Third Edition includes much-needed interpretation of the most recent ICH guidelines for validation and method development, as well as recent publications of the USP on Analytical Procedure Lifecycle Management and the activities of the British Pharmacopeia AQbD Working Party. It also addresses hot topics in the field such as data integrity and continuous monitoring of analytical performance.

Written by a team of highly qualified pharmaceutical professionals, Method Validation in Pharmaceutical Analysis includes information on relevant topics such as:

• Data governance, data integrity, and data quality, as well as analytical instrument qualification and system validation lifecycle, and continued HPLC performance qualification
• Analytical target profile, decision rules and fitness for intended use, and performance characteristics of analytical procedures
• Method selection, development, and optimization, multivariate analytical procedures, and risk assessment and analytical control strategy
• Implementation of compendial/pharmacopeia test procedures, transfer of analytical procedures, and a lifecycle approach to transfer of analytical procedures

Completely comprehensive in coverage, Method Validation in Pharmaceutical Analysis is an essential reference for scientists, researchers, and professionals in the pharmaceutical industry, analytical chemists, QC and QA staff, and public authorities tasked with relevant regulatory responsibilities....