Validation Standard Operating Procedures: A Step by Step Guide for Achieving Compliance in the Pharmaceutical, Medical Device, and Biotech Industries, Second Edition

1145 Pages·2006·12.41 MB·English

by  Syed Imtiaz Haider

Second Edition
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Second Edition
New York London
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Published in 2006 by
CRC Press
Taylor & Francis Group
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© 2006 by Taylor & Francis Group, LLC
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Library of Congress Cataloging-in-Publication Data
Haider, Syed Imtiaz.
Validation standard operating procedures : a step-by-step guide for achieving compliance in the
pharmaceutical, medical device, and biotech industries / Syed Imtiaz Haider.-- 2nd ed.
p. ; cm.
Includes bibliographical references.
ISBN-13: 978-0-8493-9529-1 (hardcover : alk. paper) ISBN-10: 0-8493-9529-1 (hardcover : alk. paper)
1. Pharmaceutical technology--Quality control. 2. Pharmaceutical industry--Standards--United States. 3.
Biotechnology industries--Standards--United States. 4. Medical instruments and apparatus
industry--Standards--United States. [DNLM: 1. Equipment Safety--standards--United States. 2. Equipment
and Supplies--standards--United States. 3. Biotechnology--standards--United States. 4. Drug
Industry--standards--United States. 5. Quality Control--United States. 6. Technology, Pharmaceutical--United
States. W 26 H149v 2006] I. Title: Step-by-step guide for achieving compliance in the pharmaceutical,
medical device, and biotech industries. II. Title.
RS192.H353 2006
681'.761'021873--dc22 2005035145
Visit the Taylor & Francis Web site at
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Taylor & Francis Group and the CRC Press Web site at
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CONTENTS
Section VAL 100.00
100.10 Introduction to Validation..................................................................3
Section VAL 200.00
200.10 Fundamentals of Validation SOPs.....................................................9
200.20 Validation Master Plan and Guideline for DQ, IQ, QQ, and PQ....14
200.30 Design Qualification Guideline for Minimizing the Risk of
Product Cross-Contamination by Air Handling System.................27
200.40 Design Qualification Guideline for Minimizing the Risk of
Cross-Contamination of Facility, Equipment, and Process...........32
200.50 Design Qualification Guideline for HVAC System of
a Pharmaceutical Plant.....................................................................37
200.60 Design Qualification for the Prevention of Contamination of
Non-Sterile Pharmaceutical Products..............................................51
200.70 Design Qualification Guideline for Cross-Contamination
and Decontamination.......................................................................54
200.80 Design Specifications for Process Water........................................60
200.90 Design Specifications for Water for Injection Production
and Distribution................................................................................72
200.100 Design Specifications for Purified Water (DIW) Production
and Distribution................................................................................86
200.110 Design Specification for Pure Steam Production
and Distribution................................................................................89
Section VAL 300.00
300.10 Validation Glossary...........................................................................95
300.20 Organization for Validation............................................................101
300.30 Revalidation.....................................................................................104
300.40 Retrospective Validation.................................................................107
300.50 Validation Change Control.............................................................110
v
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vi (cid:1) Validation Standard Operating Procedures (cid:1)
Section VAL 400.00
400.10 Calibration of Instruments.............................................................117
400.20 Periodic Review of the Calibration Program...............................126
400.30 Calibration and Validation Equipment..........................................131
Section VAL 500.00
500.10 Training on the Job........................................................................137
500.20 Good Manufacturing Practices......................................................140
Section VAL 600.00
600.10 Guidelines for Area Classification and Air Handling..................151
600.20 Guideline for Area Validation: Clean Area...................................156
600.30 Aseptic Area Validation Procedures..............................................164
600.40 Microbiological Monitoring of Areas Used for Production of
Solids, Semi-Solids, and Liquids....................................................190
600.50 Efficiency Testing for Disinfectants...............................................195
600.60 Drinking Water...............................................................................199
600.70 Purified Water.................................................................................202
600.80 Water for Injection.........................................................................205
600.90 Validation of a Water System........................................................208
600.100 Oil-Free Compressed Air System..................................................218
600.110 Nitrogen Distribution System.........................................................223
600.120 Clean Steam....................................................................................229
600.130 Vacuum System...............................................................................235
600.140 Validation of an HVAC System......................................................240
Section VAL 700.00
700.10 Validation of a Steam Sterilizer.....................................................259
700.20 Hot Air Sterilization Tunnel Certification and
Validation Guideline.......................................................................269
700.30 Freeze Drier....................................................................................285
700.40 Ampule and Vial Washing Machine..............................................293
700.50 Washing, Sterilizing, and Drying Machine for Stoppers.............297
700.60 Ampule and Vial Filling Machine.................................................304
700.70 Media Fill Run................................................................................308
700.80 Half-Automatic Inspection Machine..............................................318
700.90 Ampule Crack Detection Machine................................................321
700.100 Laminar Flow Installations.............................................................326
700.110 Sterile Filtration Validation.............................................................329
700.120 Cleaning Efficiency of Production Equipment for Parenterals...332
Section VAL 800.00
800.10 Kneading Machine..........................................................................337
800.20 Oscillating Granulator....................................................................341
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(cid:1) Validation Standard Operating Procedures (cid:1) vii
800.30 Milling Machine..............................................................................345
800.40 Fluid Bed Drier...............................................................................348
800.50 Blender............................................................................................353
800.60 Tablet Press.....................................................................................357
800.70 Metal Check Device for Tablets....................................................362
800.80 Tablet Coater...................................................................................366
Section VAL 900.00
900.10 Blistering Machine..........................................................................373
900.20 Blister Filling Machine...................................................................377
900.30 Code Reader...................................................................................381
900.40 Sachetting Machine.........................................................................384
900.50 Cartoning Machine.........................................................................388
900.60 Labeling Machine...........................................................................392
900.70 Check Weigher................................................................................396
900.80 Shrink Wrapping and Bundling Machine.....................................399
900.90 Tube Filling and Closing Machine................................................402
900.100 Liquid Filling and Closing Machine..............................................406
900.110 Tablet Filling and Closing Machine..............................................410
Section VAL 1000.00
1000.10 Installation Qualification of Computerized Equipment...............417
1000.20 Operational Qualification of Computerized Equipment.............423
1000.30 Performance Qualification of Computerized Equipment............429
Section VAL 1100.00
1100.10 Validation of Microbiological Methods.........................................435
1100.20 Validation of Analytical Methods..................................................448
Section VAL 1200.00
1200.10 Vendor Certification........................................................................461
Section VAL 1300.00
1300.10 Facility Qualification.......................................................................467
Section VAL 1400.00
1400.10 Sterilization Assurance Information and Data...........................477
Section VAL 1500.00
1500.10 Qualification and Requalification Matrix....................................543
1500.20 Vial/Ampoule Washer Performance Qualification Protocol.....550
1500.30 Vial/Ampoule Washer Performance Requalification Protocol...558
1500.40 Depyrogenation Tunnel Performance Qualification Protocol..566
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1500.50 Depyrogenation Tunnel Performance Requalification
Protocol.........................................................................................576
1500.60 SIP Cycle for Holding Vessel Requalification Protocol.............581
1500.70 Stopper Sterilization Performance Qualification Protocol........586
1500.80 Stopper Sterilization Requalification Protocol............................590
1500.90 Equipment Sterilization Performance Qualification Protocol...594
1500.100 Lyophilizer Performance Qualification Protocol........................598
1500.110 Lyophilizer Requalification Protocol...........................................609
Section VAL 1600.00
1600.10 Qualification and Requalification Summary Report..................619
1600.20 Vial/Ampoule Washer Performance Qualification Summary
Report............................................................................................621
1600.30 Vial/Ampoule Washer Requalification Summary Report...........629
1600.40 Depyrogenation Tunnel Performance Qualification
Summary Report...........................................................................636
1600.50 Depyrogenation Tunnel Performance Requalification
Summary Report...........................................................................645
1600.60 SIP Cycle for Holding Vessels Requalification Summary
Report............................................................................................651
1600.70 Stopper Sterilization Performance Qualification Summary
Report............................................................................................655
1600.80 Stopper Sterilization Requalification Summary Report..............661
1600.90 Equipment Sterilization Performance Qualification Summary
Report............................................................................................667
1600.100 Lyophilizer Performance Qualification Summary Report.........675
1600.110 Lyophilizer Requalification Summary Report.............................680
Section VAL 1700.00
1700.10 Evidence of Formal Written Procedures....................................687
1700.20 Particulate Monitoring (Nonviable) of Injectable Area.............690
1700.30 QA Responsibilities in Injectable Area.......................................702
1700.40 Particulate Matter in Injectables, USP Criteria...........................716
1700.50 Visual Inspection of Lyophilized Product Parenterals..............725
1700.60 Microbiological Monitoring of Water..........................................731
1700.70 Monitoring of Personnel Hygiene..............................................751
1700.80 Microbiological Environmental Monitoring of Injectable
Facility...........................................................................................756
1700.90 Chemical and Physical Monitoring of DI, WFI, and RO
Waters............................................................................................798
1700.100 Validation of Sterility Test...........................................................804
1700.110 Visual Inspection of Small-Volume Parenterals.........................819
1700.120 Fill Volume/Weight and Other Checks for Parenteral
Products during Filling................................................................829
1700.130 Preservative Efficacy Test............................................................834
1700.140 Disinfectant Validation.................................................................842
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Section VAL 1800.00
1800.10 Process Simulation (Media Fill) Test..........................................869
1800.20 Media-Fill Microbiological Examination.....................................904
1800.30 Process Simulation (Media Fill) Test Protocol...........................912
1800.40 Media-Fill Run Report..................................................................926
Section VAL 1900.00
1900.10 Determination of Components Bioburden before
Sterilization...................................................................................943
1900.20 Sterility Test Results Failure Investigation..................................954
1900.30 Bacterial Endotoxin Determination in WFI, In-Process, and
Finished Products.........................................................................957
1900.40 Monitoring the Bioburden, Spore Bioburden, and Endotoxin
Present on Stoppers and Unprocessed Vials.............................967
Section VAL 2000.00
2000.10 Technical Training........................................................................981
Section VAL 2100.00
2100.10 Environmental Performance Test Procedure.............................989
2100.20 HEPA Filters Leak Test (DOP) Procedure..................................993
2100.30 Temperature Control Test Procedure.........................................997
2100.40 Airflow and Uniformity Test Procedure...................................1001
2100.50 Pressure Control Test Procedure..............................................1005
2100.60 Particulate Count Test Procedure.............................................1009
2100.70 Humidity Control Test Procedure.............................................1013
2100.80 Recovery Test Procedure...........................................................1017
2100.90 Particulate Dispersion Test Procedure.....................................1021
2100.100 Airflow Pattern Test Procedure.................................................1025
2100.110 Critical Sampling Point Determination in Cleanroom
(Viable Count)............................................................................1029
2100.120 Critical Sampling Point Determination in Cleanroom
(Nonviable Count) by Grid Method.........................................1035
Section VAL 2200.00
2200.10 Cleaning Validation Protocol of Solution Preparation Tank...1045
2200.20 Cleaning Validation Protocol of Mobile Tank..........................1059
2200.30 Cleaning Validation Protocol of Filtration Assembly...............1072
2200.40 Cleaning Validation Protocol of Freeze Dryer.........................1084
2200.50 Cleaning Validation Protocol of Vial-Filling Machine Parts....1097
Section VAL 2300.00
2300.10 Recommended Reading..............................................................1115