Second Edition. New York London

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4 Second Edition New York London

5 Published in 2006 by CRC Press Taylor & Francis Group 6000 Broken Sound Parkway NW, Suite 300 Boca Raton, FL by Taylor & Francis Group, LLC CRC Press is an imprint of Taylor & Francis Group No claim to original U.S. Government works Printed in the United States of America on acid-free paper International Standard Book Number-10: (Hardcover) International Standard Book Number-13: (Hardcover) Library of Congress Card Number This book contains information obtained from authentic and highly regarded sources. Reprinted material is quoted with permission, and sources are indicated. A wide variety of references are listed. Reasonable efforts have been made to publish reliable data and information, but the author and the publisher cannot assume responsibility for the validity of all materials or for the consequences of their use. No part of this book may be reprinted, reproduced, transmitted, or utilized in any form by any electronic, mechanical, or other means, now known or hereafter invented, including photocopying, microfilming, and recording, or in any information storage or retrieval system, without written permission from the publishers. For permission to photocopy or use material electronically from this work, please access ( or contact the Copyright Clearance Center, Inc. (CCC) 222 Rosewood Drive, Danvers, MA 01923, CCC is a not-for-profit organization that provides licenses and registration for a variety of users. For organizations that have been granted a photocopy license by the CCC, a separate system of payment has been arranged. Trademark Notice: Product or corporate names may be trademarks or registered trademarks, and are used only for identification and explanation without intent to infringe. 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: (hardcover : alk. paper) ISBN-10: (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.H '.761' dc Visit the Taylor & Francis Web site at Taylor & Francis Group is the Academic Division of Informa plc. and the CRC Press Web site at

6 CONTENTS Section VAL Introduction to Validation... 3 Section VAL Fundamentals of Validation SOPs Validation Master Plan and Guideline for DQ, IQ, QQ, and PQ Design Qualification Guideline for Minimizing the Risk of Product Cross-Contamination by Air Handling System Design Qualification Guideline for Minimizing the Risk of Cross-Contamination of Facility, Equipment, and Process Design Qualification Guideline for HVAC System of a Pharmaceutical Plant Design Qualification for the Prevention of Contamination of Non-Sterile Pharmaceutical Products Design Qualification Guideline for Cross-Contamination and Decontamination Design Specifications for Process Water Design Specifications for Water for Injection Production and Distribution Design Specifications for Purified Water (DIW) Production and Distribution Design Specification for Pure Steam Production and Distribution Section VAL Validation Glossary Organization for Validation Revalidation Retrospective Validation Validation Change Control v

7 vi Validation Standard Operating Procedures Section VAL Calibration of Instruments Periodic Review of the Calibration Program Calibration and Validation Equipment Section VAL Training on the Job Good Manufacturing Practices Section VAL Guidelines for Area Classification and Air Handling Guideline for Area Validation: Clean Area Aseptic Area Validation Procedures Microbiological Monitoring of Areas Used for Production of Solids, Semi-Solids, and Liquids Efficiency Testing for Disinfectants Drinking Water Purified Water Water for Injection Validation of a Water System Oil-Free Compressed Air System Nitrogen Distribution System Clean Steam Vacuum System Validation of an HVAC System Section VAL Validation of a Steam Sterilizer Hot Air Sterilization Tunnel Certification and Validation Guideline Freeze Drier Ampule and Vial Washing Machine Washing, Sterilizing, and Drying Machine for Stoppers Ampule and Vial Filling Machine Media Fill Run Half-Automatic Inspection Machine Ampule Crack Detection Machine Laminar Flow Installations Sterile Filtration Validation Cleaning Efficiency of Production Equipment for Parenterals Section VAL Kneading Machine Oscillating Granulator

8 Validation Standard Operating Procedures vii Milling Machine Fluid Bed Drier Blender Tablet Press Metal Check Device for Tablets Tablet Coater Section VAL Blistering Machine Blister Filling Machine Code Reader Sachetting Machine Cartoning Machine Labeling Machine Check Weigher Shrink Wrapping and Bundling Machine Tube Filling and Closing Machine Liquid Filling and Closing Machine Tablet Filling and Closing Machine Section VAL Installation Qualification of Computerized Equipment Operational Qualification of Computerized Equipment Performance Qualification of Computerized Equipment Section VAL Validation of Microbiological Methods Validation of Analytical Methods Section VAL Vendor Certification Section VAL Facility Qualification Section VAL Sterilization Assurance Information and Data Section VAL Qualification and Requalification Matrix Vial/Ampoule Washer Performance Qualification Protocol Vial/Ampoule Washer Performance Requalification Protocol Depyrogenation Tunnel Performance Qualification Protocol.. 566

9 viii Validation Standard Operating Procedures Depyrogenation Tunnel Performance Requalification Protocol SIP Cycle for Holding Vessel Requalification Protocol Stopper Sterilization Performance Qualification Protocol Stopper Sterilization Requalification Protocol Equipment Sterilization Performance Qualification Protocol Lyophilizer Performance Qualification Protocol Lyophilizer Requalification Protocol Section VAL Qualification and Requalification Summary Report Vial/Ampoule Washer Performance Qualification Summary Report Vial/Ampoule Washer Requalification Summary Report Depyrogenation Tunnel Performance Qualification Summary Report Depyrogenation Tunnel Performance Requalification Summary Report SIP Cycle for Holding Vessels Requalification Summary Report Stopper Sterilization Performance Qualification Summary Report Stopper Sterilization Requalification Summary Report Equipment Sterilization Performance Qualification Summary Report Lyophilizer Performance Qualification Summary Report Lyophilizer Requalification Summary Report Section VAL Evidence of Formal Written Procedures Particulate Monitoring (Nonviable) of Injectable Area QA Responsibilities in Injectable Area Particulate Matter in Injectables, USP Criteria Visual Inspection of Lyophilized Product Parenterals Microbiological Monitoring of Water Monitoring of Personnel Hygiene Microbiological Environmental Monitoring of Injectable Facility Chemical and Physical Monitoring of DI, WFI, and RO Waters Validation of Sterility Test Visual Inspection of Small-Volume Parenterals Fill Volume/Weight and Other Checks for Parenteral Products during Filling Preservative Efficacy Test Disinfectant Validation

10 Validation Standard Operating Procedures ix Section VAL Process Simulation (Media Fill) Test Media-Fill Microbiological Examination Process Simulation (Media Fill) Test Protocol Media-Fill Run Report Section VAL Determination of Components Bioburden before Sterilization Sterility Test Results Failure Investigation Bacterial Endotoxin Determination in WFI, In-Process, and Finished Products Monitoring the Bioburden, Spore Bioburden, and Endotoxin Present on Stoppers and Unprocessed Vials Section VAL Technical Training Section VAL Environmental Performance Test Procedure HEPA Filters Leak Test (DOP) Procedure Temperature Control Test Procedure Airflow and Uniformity Test Procedure Pressure Control Test Procedure Particulate Count Test Procedure Humidity Control Test Procedure Recovery Test Procedure Particulate Dispersion Test Procedure Airflow Pattern Test Procedure Critical Sampling Point Determination in Cleanroom (Viable Count) Critical Sampling Point Determination in Cleanroom (Nonviable Count) by Grid Method Section VAL Cleaning Validation Protocol of Solution Preparation Tank Cleaning Validation Protocol of Mobile Tank Cleaning Validation Protocol of Filtration Assembly Cleaning Validation Protocol of Freeze Dryer Cleaning Validation Protocol of Vial-Filling Machine Parts Section VAL Recommended Reading

12 PREFACE As the validation master plan execution program proceeds and the facility is integrated into regulatory guidelines of the FDA, current good manufacturing practices (cgmps), good laboratory practices (GLPs), and the need for comprehensive and well-defined validation supporting standard operating procedures (SOPs) are required. As the validation program progresses and the systems are integrated into routine operation, there are fewer deviations and the SOPs become more precise and complete. This book and CD-ROM provide an administrative solution for management. The execution of test functions defined in the validation master plan procedures is provided in the text and the electronic files. The validation standard operating procedure can help your company comply with GMP, GLP, and validation requirements imposed by the FDA. The formats and style provided are generic and can be further amended. The contents of the SOPs are intended to build quality into the regulatory requirements. However, having a set of validation SOPs does not preclude adverse inspection findings because contents that satisfy one inspector may not satisfy another. I strongly believe that the facility s technical management and staff should read the procedures to ensure that particular needs are addressed with reference to operational control within the organization and individual countries regulatory requirements. It is, however, guaranteed to provide management with a tool to develop a set of validation SOPs in order to support the road map established for the on-time successful start-up of the facility operation in compliance with the GMP requirement. The pharmaceutical industry and its top management are confronted today with a period in which the demands for validation, GMP, and GLP compliance have never been greater. The validation procedures in the present environment must be designed to ensure regulatory compliance xi

13 xii Validation Standard Operating Procedures in pharmaceutical operations as well as serve as a training source for undergraduates and graduates at the academic level. The first edition comprised Val. Section 200 to Val. Section 1300, providing 75 validation SOPs covering design qualification, utilities qualification, facility qualification, equipment qualification, training needs, and major sterile and nonsterile operations-related equipment. In Val. Section 1400 to Val. Section 2300, the second edition provides additional information needed to respond to increasing demand by official regulatory bodies worldwide. I have assembled a matrix that will provide a source for experienced and inexperienced practitioners in the pharmaceutical, biotech, and medical device industries. In the second edition, 64 new validation SOPs are added to describe documentation required for sterility assurance, qualification and requalification template reports of major sterile equipments, critical applicable procedures, templates for certification guidelines, media fill procedures, environmental control guidelines, training, and critical environmental performance evaluation procedures. The second volume provides 139 template procedures, protocols, and reports that can be downloaded and, after minor changes, adopted. The ready-to-use protocols allow end users to record all raw hard data, further enabling them to prepare final reports. The additional chapters included in this edition provide details on how to ensure sterility and prepare sterility assurance reports. Section Val provides a unique template on how to prepare and submit sterility assurance and information data for submission to FDA in ANDA and NDA submissions. Section Val provides 11 state-of-the-art validation protocols covering critical aseptic processing equipment. Section Val describes 11 examples of how to prepare critical qualification and requalification reports related to aseptic operations and provides them as a proof of records to FDA for ANDA and ANDA file submissions. Section Val provides 14 exclusive procedures describing critical monitoring operations to ensure sterility assurance. Comprehensive process simulation (media fill) test, media fill microbial examination, process simulation test protocol and template media fill run reports are provided in Section Val Section Val includes four aseptic processes associated with monitoring and qualification programs covering determination of components bioburden before sterilization sterility test failure investigation, bacterial endotoxin determination in WFI, in-process finished product, and monitoring the bioburden, spore bioburden, and endotoxin present on stoppers and unprocessed vials.

14 Validation Standard Operating Procedures xiii Section Val describes the training needs of personnel involved in aseptic operations. Section Val provides 14 critical environmental performance evaluation tests, including: Five discrete cleaning validation protocols related to aseptic manufacturing equipments, solution preparation tanks, mobile tanks, filtration assemblies, freeze dryers, and vial filling machine parts are provided in Section Val Section Val includes recommended reading. Pharmaceutical, medical, and biotech industries are regulated worldwide to be in compliance with cgmp and GLP principles. Each company is required to create validation SOPs to qualify its equipment, utilities, buildings, and personnel. The template validation SOPs available enable end users to understand principles and elements of good manufacturing practice and provide documentation language ranging from generic to specific, depending on the detail level of the requirements. Compliance to FDA regulations by the health care industry over the last decade has been a major goal, including those companies intending to export their product to the U.S. market. As a result, only a few companies are able to seek approval for exportation; one of the reasons behind this is the absence or inadequacy of validation SOPs. The validation SOPs on the CD-ROM are valuable tools for companies in the process of developing or revising validation SOPs to achieve FDA, GMP, and GLP compliance. The documentation package is especially relevant to quality assurance personnel, engineers, utilities engineers, computer engineers, validation designers, internal and external auditors, or to anyone interested in developing a qualification documentation matrix. Syed Imtiaz Haider

16 DEDICATION This book is dedicated to my loving father Syed Mohsin Raza, and to my late mother, Syeda Kharsheed-un-Nissan, for their continuous motivation. I am also indebted to my wife, Syeda Shazia Fatima, my son, Syed Zeeshan Haider, and my daughter, Syeda Mehreen Fatima, for their patience while I compiled this book. xv

18 ACKNOWLEDGMENTS I am thankful to Mr. Abdul Razzaq Yousef, the managing director of Gulf Pharmaceutical Industries, for always encouraging me on my professional achievements and continuously keeping me motivated. I would also like to thank my friends and colleagues Ateeq Hashmi and Javed Zamir for their help and encouragement and for creating a professional environment. Special thanks to the staff of Taylor & Francis Books for their patience and diligence in the production of this book. xvii

20 THE AUTHOR Syed Imtiaz Haider earned his Ph.D. in chemistry and is a quality assurance and environmental specialist with over 15 years of experience in aseptic and nonaseptic pharmaceutical processes, equipment validation, and in-process control and auditing. Dr. Haider is the author and coauthor of more than 20 research publications in international refereed journals dealing with products of pharmaceutical interest, their isolation, and structure development. A professional technical writer, Dr. Haider has authored more than 2000 standard operating procedures based on FDA regulations, ISO 9001:2000, and ISO 14001:2004 standards. He is a certified QMS auditor of IRCA and registered associate environmental auditor of EARA. He has written more than ten quality system manuals for multidisciplinary industries and provided consultancy to the Ministry of Health, United Arab Emirates, Drug Control Laboratory, in developing a quality management system based on ISO 9003 and later transition to ISO 9001:2000. Dr. Haider is working as a quality affairs director at Julphar, Gulf Pharmaceutical Industries, and is involved in the preparation of several abbreviated new drug application (ANDA) files, followed by successful FDA, EU GMP inspections leading to export of finished pharmaceutical products to the U.S. and European markets. He has also written ISO 9001: 2000: Document Development Compliance Manual: A Complete Guide and CD-Rom and Pharmaceutical Validation Master Plan, The Ultimate Guide to FDA, GMP, and GLP Compliance. Dr. Haider holds the intellectual copyright certificate of registration on an electronic documentation package on ISO 9000 and ISO from the Canadian Intellectual Property Office. He is also a contributing author of chapters on ISO 9001: 2000 and ISO in international publications. xix

FDA s Guidance for Industry

FDA s Guidance for Industry Sterile Drug Products Produced by Aseptic Processing - CGMPs Midwest FDC Conference November 4 2005 Susan Bruederle, Investigator FDA / ORA / Central Region Chicago District / Hinsdale IL FDA s Guidance