Pharmaceutical Calibration, Validation and Qualification: A Comprehensive Approach

Preface
Contents
About the Editors
Part I: Calibration
Chapter 1: Introduction to Calibration
Introduction
Definition
Purpose of Calibration [2] (Fig. 1.1)
Need of Calibration (Fig. 1.2)
Benefits of Calibration
Traceability
Test Accuracy Ratio (TAR)
Types of Calibration
Parameters to be Calibrated
Calibration Techniques and Methods
Methods of Calibration
Calibration in Analytical Measurements
Process of Calibration
A Successful Calibration Procedure Requires the Following Basic Steps
Calibration Personnel
Calibration Laboratory
Calibration Certificate and Report
Recalibration
Factors Influencing Recalibration
Conclusion
References
Chapter 2: Errors and Uncertainties in Calibration
Introduction
Error and Its Types
Calibration and Its Types
Types of Calibration
Definition of Uncertainty
Difference Between Error and Uncertainty
Sources of Uncertainty
Calculation of Uncertainty
Methods of Uncertainty Analysis
Type A Evaluations
Type B Evaluations
Methods of Uncertainty Analysis
Design-Stage Uncertainty Analysis
Zero Order Uncertainty
Sequential Perturbation
Conclusion
References
Chapter 3: Calibration Methods and Procedures
Introduction
Calibration Process
Steps for Calibration Determination
Selection of Calibration Method
Procedure of Calibration
Pressure Calibration
Temperature Calibration
Flow Calibration
Pipette Calibration
Electrical Calibration
Mechanical Calibration
Key Requirements for Calibration Process
Calibration Frequency
Sources of Calibration
Calibration Laboratory
Calibration Based on Types of Instrument
Linear Instruments
Nonlinear Instruments
Discrete Instruments
Uncertainty Estimation
Conclusion
References
Chapter 4: Calibration Software Support
Introduction
Difference Between Calibration and Maintenance
Calibration Management Software
Need of Calibration Management Software
Types of Calibration Software
Conclusion
References
Part II: Qualification
Chapter 5: Objectives of Qualification
Introduction
Objectives of Qualification
Benefits of Qualification
Need/Requirement of Qualification
Difference between Validation, Calibration, and Qualification
Relationship Between Validation, Calibration, and Qualification
Types of Equipment
Critical Equipment
Non-critical Equipment
Life Cycle of Equipment and Steps for Qualification of Equipment
Phases/Elements of Qualification
Specification Phase
Verification Phase
Phase I
Phase-II
Operational Qualification (OQ)
Performance Qualification (PQ)
Preventive Maintenance and Repairs
Routine Practices for Operation, Calibration, Maintenance, and Change Control
Other Miscellaneous Qualification
Acceptance Criteria
Regulatory Requirements
Conclusion
References
Chapter 6: Approach to the Qualification Process
Introduction
Approaches to Qualification Process
Purpose
Quality Risk Management Approach [QRM]
Steps of QRM Approach
Recommendations
Acceptable Analytical Practices
General Requirements to Set AAPs
Equipment Maintenance
Computers and Software Used to Control Equipment
Qualification Life Cycle Approach
Regulatory Environment
New ECA AQCG Guideline on Analytical Procedure Lifecycle Management (APLM)
Process Performance Qualification Approach
The Right Place to Begin
Defining the Risk
Determining Regulatory Starting Material(s) and Campaign Strategies
Pre-PPQ
Establishing the Protocol
Pre-approval Inspection
The Final Report
Conclusion
References
Part III: Verification
Chapter 7: Objectives, Methods, and Role of Verification
Introduction
Definition of Verification
Objectives of Verification (Fig. 7.1)
Purpose of Verification
Difference Between Verification versus Validation
System Verification
Classification of Verification
Approaches to Verification
Methods of Verification
Inspection/Examination
Demonstration
Test
Analysis
Verification Process
Step 1: Verification Planning
Step 2: Verification Execution
Step 3: Verification Reporting
Software Verification
Methods of Software Verification
Peer Reviews/Informal Reviews
Walkthrough/Semiformal Reviews
Inspections/Formal Review
Rules of Review
Categories of Verification
Dynamic Testing
Functional Testing
Structural Testing
Random Testing
Static Testing
Static and Dynamic Verification
Verification and Validation Goals
Types of Testing
Testing and Debugging
V&V Planning
Conclusion
References
Chapter 8: Improvement in Software Quality
Introduction
Software Quality Assurance (SQA)
Software Quality Control (SQC)
Testing
Areas for Step Up in Software Quality
Deming Wheel (PDCA Cycle) (Fig. 8.1)
Key Rudiments and Meters for Progress in Software Quality
Devising a Plan and Defining Strategy
Quality Management Plan
Test Strategy
Scenario Analysis
Test Data Identification
Models for Improvement in Software Quality
Steps for Improvement in Software Quality
Test Early and Test Often with Automation
Requirement Specification Document Availability
Testing Team Concern in Requirement Discussions
Clear-Cut Scope
Test Planning and Execution
Test Case Review
Regression Test Planning
Importance of Regression Testing (Fig. 8.11)
Different Ways to Perform Regression Testing
Test Data Management and Reporting
Retrospection After Every Sprint
Conclusion
References
Part IV: Validation
Chapter 9: General Principles of Validation
Introduction
Definitions of Validation
According to European Commission
According to US FDA Definition
According to ICH Definition
According to WHO Definition
Need/Purpose of Validation
Principles of Validation
Validation Master Plan
Validation Protocol
Validation Summary Report
Validation Setup
Roles and Responsibilities of Validation Team (Table 9.1)
Validation Life Cycle
Conclusion
References
Chapter 10: Process Validation and Its Types
Introduction
Definition of the Term ``Validation´´
Definition of the Term ``Process´´
Process Validation
Definition of Process Validation
Process Optimization
Types of Process Validation
Prospective Validation (or Premarket Validation)
Criteria for Prospective Validation
Concurrent Validation
When Concurrent Validation is Carried Out?
Retrospective Validation
Revalidation
Regulatory Requirements for Process Validation
Requirements of ISO 13485
Further Relevant National and International Provisions
Requirements of the FDA
Requirements of the WHO
Order of Priority in Process Validation
Documentation
Process Validation of Various Dosage Forms
Manufacturing Process
Process Control
Responsibilities of Process Validation Team Product [9] (Fig 10.1)
Conclusion
References
Part V: Analytical Validation
Chapter 11: Pharmaceutical Equipment Validation
Introduction
Types of Validation
Equipment Validation
Types of Equipment Validation
Phases of Equipment Validation
Pre-validation Phase
Design Qualification (DQ)
Installation Qualifications (IQ)
Process Validation Phase
Operational Qualifications
Performance Qualification
Revalidation
Validation Maintenance Phase
Applications of Equipment Validation
References
Chapter 12: Cleaning Validation for the Pharmaceutical, Biopharmaceutical, and Nutraceuticals
Introduction
Cleaning Validation
Objective
Need for Cleaning Validation
Why Cleaning Validation [1]
In Case of Drug Products
Level 1 Cleaning
Level 2 Cleaning
Cleaning Validation Master Plan
Elements of Cleaning Validation
Residue Identification
Equipment Characterization
Cleaning Agent Selection
TACT
WINS
Grouping of Equipment
Product Grouping and Equipment Grouping
Grouping for Products
Cleaning Procedures
Sampling Technique
Direct Surface Sampling
Swab Sampling
Rinse Sampling
Placebo Sampling
Analytical Techniques
Additional Techniques
Validation Protocols
Background
Validation Reports
Conclusion
References
Part VI: Validation of Dosage Forms
Chapter 13: Validation of Pharmaceutical Dosage Forms
Introduction
Directives for Process Validation of Solid Dosage Forms
Protocol for Process Validation
Steps for Validation and Acceptance Criteria
Industrial Process Assessment and Selection for Tablets
Determination of the Unit Operations Required to Fabricate the Tablets Is as Follows
Mixing or Blending
Wet Granulation
Wet Milling
Drying
Milling
Lubrication (Fig. 13.6)
Tablet Compression
Tablet Coating
In-Process Quality Control Tests (IPQC)
Objectives of In-Process Quality Control
The Following Figure Depicts the Objectives of IPQC (Fig. 13.9)
Change Control
Documentation
Process Validation of Capsules [19]
Capsule Shell Contents
Speed of Encapsulation
Encapsulation
Validation of Liquids [20, 21]
Validation Includes Mainly Following Tests
Monitoring Outputs
Process Validation of Semisolid Dosages Forms [22, 23]
Critical Parameters to Be Validated
Conclusion
References
Part VII: Validation of Herbals
Chapter 14: Approach for Herbal Standardization
Introduction
Approaches in Herbal Drug Standardization
DNA Fingerprinting
Chromatographic Fingerprinting
Biopharmaceutical Characterization of Herbal Medicinal Products
Relevance of the Biopharmaceutical Classification System for HMPs
Determination of the Solubility of Extracts and Active Markers in BCS-Buffers
EMEA (European Agency for the Evaluation of Medicinal Products) Guidelines for Evaluation of Herbal Medicines (EMEA, 2820/00)
Tablets (Coated and Uncoated) and Hard Capsules
Chemistry-Manufacturing-Control (CMC) Considerations for Herbal Products
Conclusion
References
Chapter 15: Regulatory Requirements for Herbal Medicines in India
Introduction
Herbal Medicines
Indian Regulations
Ministry of AYUSH
Objective of AYUSH
AYUSH Certification
Drug Development Process of Herbal Medicines
Clinical Trials of Herbal Medicines
Stages of Clinical Trial (Fig. 15.5)
Guidelines for Good Clinical Practice for Herbal Drugs and Products in Conducting Clinical Trials in India
Conclusion
References
Part VIII: Expert Opinion
Chapter 16: Expert Opinion on the Basis of Table of Contents