Method Validation in Pharmaceutical Analysis : A Guide to Best Practice

• Autore: Ermer Joachim
• Pubblicazione: Newark : , : John Wiley & Sons, Incorporated, , 2025; ©2025
• Edizione: 3rd ed.
• Descrizione fisica: 1 online resource (542 pages)
• Disciplina: 615.1901
• Altri autori: NethercotePhil W
• Nota di contenuto: Cover -- Title Page -- Copyright -- Contents -- Preface -- Chapter 1 Analytical Validation Within the Pharmaceutical Lifecycle -- 1.1 Development of Process and Analytical Validation Concepts -- 1.2 Alignments Between Process and Analytics: Three‐Stage Approach -- 1.3 Predefined Objectives: ATP -- 1.4 Analytical Lifecycle -- References -- Part I Prerequisites -- Chapter 2 Data Governance, Data Integrity, and Data Quality -- 2.1 Terminology Used in This Chapter -- 2.1.1 Data Governance -- 2.1.2 Data Integrity -- 2.1.3 Data Quality -- 2.2 Data Governance and Data Integrity Model -- 2.2.1 Descriptions of the Four Levels in the Model -- 2.2.2 Foundation - Data Governance -- 2.2.2.1 Senior Management Involvement -- 2.2.2.2 Policies and Procedures Need To Be in Place -- 2.2.2.3 Roles and Responsibilities -- 2.2.2.4 Quality Culture and Working Environment -- 2.2.2.5 Outsourcing Analysis -- 2.2.2.6 Quality Oversight -- 2.2.3 Level 1: Analytical Instrument Qualification and System Validation (AIQSV) -- 2.2.4 Level 2: Analytical Procedure Lifecycle -- 2.2.5 Level 3: Right Analysis for the Right Analytical Result -- 2.2.6 Quality Oversight for Data Integrity -- 2.3 Interaction Between Levels 1 and 2 -- 2.4 Overview of Data Integrity -- 2.5 ALCOA Criteria for Data Integrity -- 2.6 Understanding Level 3: Right Analysis for the Right Reportable Result -- 2.6.1 Analytical Procedure -- 2.6.2 Trained Analysts Working in an Open Culture -- 2.6.3 Instruments and Systems Used -- 2.6.4 Sample Preparation -- 2.6.5 Time Synchronisation -- 2.6.6 Digitalisation of Sample Preparation -- 2.6.7 Instrumental Analysis by Chromatography -- 2.6.8 Peak Integration -- 2.6.9 Calculation of the Reportable Result -- 2.7 Second‐Person Review -- 2.8 Summary -- References -- Chapter 3 Analytical Instrument Qualification and System Validation Lifecycle. ; 3.1 Data Integrity and Data Quality in a GMP Environment -- 3.1.1 Criteria for Data Quality -- 3.1.2 Regulatory Rationale for Qualified Analytical Instruments and Validated Systems -- 3.2 AIQSV Approach as an Essential Part of the Analytical Procedure Lifecycle -- 3.3 USP General Chapter < -- 1058> -- -- 3.3.1 Data Quality Triangle -- 3.3.2 AIQ Lifecycle: The 4Qs Model -- 3.3.3 Risk‐Based Classification of Apparatus, Instruments, and Systems -- 3.3.4 Roles and Responsibilities for AIQ -- 3.3.5 Software Validation for Group B and C Systems -- 3.4 Enhancement of < -- 1058> -- and Harmonization of a Risk‐Based Approach to Instruments and Systems with GAMP -- 3.4.1 Increased Granularity of USP < -- 1058> -- Groups -- 3.4.2 Clarification of AIQ Terminology -- 3.4.3 A Continuum of Analytical Apparatus, Instruments, and Systems -- 3.4.4 Mapping USP < -- 1058> -- Instrument Groups to GAMP Software Categories -- 3.4.5 Enhanced Data Quality Triangle -- 3.5 Risk‐Based Approaches to Analytical Instrument and System Qualification -- 3.5.1 Expanded < -- 1058> -- Instrument and System Categories -- 3.5.1.1 Group A - Apparatus -- 3.5.1.2 Group B - Instruments -- 3.5.1.3 Group C - Systems -- 3.5.2 Examples of Possible Lifecycle Activities for the Eight Enhanced Categories -- References -- Chapter 4 Continued HPLC Performance Qualification -- 4.1 Introduction -- 4.1.1 The Importance of Analytical Instrument Qualification -- 4.1.2 Terms and Definitions -- 4.1.3 Continued Performance Qualification: More by Less -- 4.2 Development of the Revised OQ/PQ Parameters List -- 4.3 Transfer of Modular Parameters into the Holistic Approach -- 4.3.1 Autosampler -- 4.3.2 Solvent Delivery System -- 4.3.3 Detector -- 4.4 OQ/PQ Data in Comparison with SST Data -- 4.5 Performance Monitoring: Trending Plots/Control Charts -- 4.5.1 Automated Limit Checking. ; 4.6 General Procedure for cPQ -- 4.7 Example -- 4.8 Concluding Remarks -- Acknowledgment -- References -- Part II Establishment of Measurement Requirements -- Chapter 5 Analytical Target Profile -- 5.1 Introduction -- 5.2 Components of an ATP -- 5.3 The Probability Statements -- 5.4 Metrics for Assessment -- 5.5 Summary -- Acknowledgments -- References -- Chapter 6 Decision Rules and Fitness for Intended Purpose -- 6.1 Introduction -- 6.2 Defining the Fitness for Intended Purpose -- 6.3 Decision Rules -- 6.4 Overview of Process to Develop Requirements for Procedure Performance -- 6.5 Decision Rules and Compliance -- 6.6 Calculating Target Measurement Uncertainty -- 6.6.1 Coverage Factor, k, and Data Distributions -- 6.7 Types of Decision Rules -- 6.7.1 Decision Rules That Use Guard Bands -- 6.7.2 Decision Rules That Use Transition Rules -- 6.8 Target Measurement Uncertainty in the ATP -- 6.8.1 Cost of Analysis -- 6.9 Bias and Uncertainty in a Procedure -- 6.10 ATP and Key Performance Indicators -- 6.11 Measurement Uncertainty -- 6.11.1 What Uncertainty Is -- 6.11.2 Reporting Measurement Uncertainty -- 6.11.3 How Uncertainty Is Estimated -- 6.11.3.1 Step 1. Specify the Measurand -- 6.11.3.2 Step 2. Identify Uncertainty Components and Data Sources -- 6.11.3.3 Step 3. Quantify the Uncertainty Components -- 6.11.3.4 Step 4. Calculate the Combined Uncertainty -- 6.11.3.5 Step 5. Calculate the Expanded Uncertainty -- 6.11.4 Uncertainty Contains All Sources of Random Variability -- 6.12 Example -- 6.13 Conclusion -- References -- Chapter 7 Performance Characteristics of Analytical Procedures -- 7.1 Precision -- 7.1.1 The Normal Distribution and its Parameters -- 7.1.1.1 But How Do I Know that My Analysis Results Are Normally Distributed? -- 7.1.1.2 So Why Is the Normal Distribution that Popular? -- 7.1.1.3 Student‐t‐Distribution. ; 7.1.1.4 Confidence Intervals -- 7.1.2 The Log‐normal Distribution -- 7.1.3 Normal, Not‐normal, and Out‐of Specification (OOS) -- 7.1.3.1 Out‐of‐Specification (OOS) Results -- 7.1.4 Precision Levels -- 7.1.4.1 System or Instrument Precision -- 7.1.4.2 Repeatability -- 7.1.4.3 Intermediate Precision and Reproducibility -- 7.1.4.4 Precision of the Reportable Result -- 7.1.5 Calculation of Precisions and Variances -- 7.1.5.1 Analysis of Variances (ANOVA) -- 7.1.5.2 Calculation of Precision from Linear Regression -- 7.1.5.3 Measurement Uncertainty (Error Propagation) -- 7.1.6 Concentration Dependency of Precision -- 7.1.7 Precision Acceptance Criteria -- 7.1.7.1 Acceptable Precision for Assay -- 7.1.7.2 Acceptable Precision for Impurities and Minor Components -- 7.1.7.3 Precisions Benchmarks -- 7.1.8 Precision and Reportable Range -- 7.1.9 Precision Highlights -- 7.2 Accuracy -- 7.2.1 Inference from Precision, Response, and Specificity -- 7.2.2 Comparison -- 7.2.2.1 Significance Tests -- 7.2.2.2 Equivalence Tests -- 7.2.2.3 Direct Comparison (Point Estimate) -- 7.2.2.4 Comparison Examples -- 7.2.3 Spiking Studies (Recovery) -- 7.2.3.1 Percentage Recovery -- 7.2.3.2 Recovery Function -- 7.2.3.3 Standard Addition -- 7.2.3.4 Impurities/Degradants -- 7.2.4 Combined Evaluation of Accuracy and Precision -- 7.2.5 Acceptance Criteria -- 7.2.6 Stability of Sample and Reference Standard Solutions -- 7.2.7 Accuracy Highlights -- 7.3 Specificity/Selectivity -- 7.3.1 Selective Detection -- 7.3.2 Selective Sample Preparation -- 7.3.3 Stress Samples -- 7.3.4 Demonstration of Specificity/selectivity by Accuracy -- 7.3.5 Chromatographic Resolution -- 7.3.6 Peak Purity (Co‐elution) -- 7.3.6.1 Re‐chromatography -- 7.3.6.2 Diode Array Detection -- 7.3.6.3 LC‐MS -- 7.3.7 Specificity/selectivity Highlights -- 7.4 Response (Calibration Model). ; 7.4.1 Unweighted Linear Regression -- 7.4.1.1 Prerequisites -- 7.4.1.2 Confidence and Prediction Intervals -- 7.4.1.3 Graphical Evaluation of the Calibration Model -- 7.4.1.4 Numerical Regression Parameters -- 7.4.1.5 Statistical Linearity Tests -- 7.4.1.6 Evaluation of the Intercept (Absence of Systematic Errors) -- 7.4.2 Weighted Linear Regression -- 7.4.3 Appropriate Calibration Models -- 7.4.3.1 Optimal Concentration for Single‐point Calibration in Case of Impurity Testing -- 7.4.3.2 Area% Quantitation -- 7.4.3.3 Matrix Impact -- 7.4.4 Non‐linear Response -- 7.4.5 Calibration Highlights -- 7.5 Detection and Quantitation Limits -- 7.5.1 Requirements in Pharmaceutical Impurity Determination -- 7.5.1.1 General Quantitation Limit -- 7.5.1.2 Intermediate Quantitation Limit -- 7.5.2 Approaches Based on the Blank -- 7.5.3 Determination of DL/QL from Linear Response -- 7.5.3.1 Standard Deviation of the Response -- 7.5.3.2 95% Prediction Interval of the Regression Line -- 7.5.3.3 Approach Based on German Standard DIN 32645 -- 7.5.3.4 From the Relative Uncertainty -- 7.5.4 Accuracy and Precision‐based Approaches -- 7.5.5 Comparison of the Various Approaches -- 7.5.6 Quantitation Limit Highlights -- Acknowledgments -- References -- Part III Method Design and Understanding -- Chapter 8 ICHQ14 Analytical Procedure Development -- 8.1 Introduction -- 8.2 The ATP -- 8.3 Connection Between Product and Analytical Procedure Understanding -- 8.4 Prior and Platform Knowledge -- 8.5 Robustness and Method Operable Design Region (MODR) -- 8.6 Link and Impact with Analytical Procedure Validation -- 8.7 Analytical Procedure Control Strategy and Ongoing Procedure Performance Verification -- 8.8 Lifecycle Strategy Including Enhanced Approaches in Submission -- 8.9 Summary -- References -- Chapter 9 Method Selection, Development, and Optimization -- 9.1 Introduction. ; 9.2 Method Selection.
• Sommario/riassunto: 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.
• Titolo autorizzato: Method Validation in Pharmaceutical Analysis
• ISBN: 9783527831715; 3527831711; 9783527831708; 3527831703; 9783527831692; 352783169X
• Formato: Materiale a stampa
• Livello bibliografico: Monografia
• Lingua di pubblicazione: Inglese
• Record Nr.: 9911019522803321
• Lo trovi qui: Univ. Federico II