SPECIFICATION OF DRUG SUBSTANCES AND PRODUCTS DEVELOPMENT AND VALIDATION OF ANALYTICAL METHODS Edited by Christopher M. Riley, Riley and Rabel Consulting Services, Maryville, MO, USA Thomas W. Rosanske, T.W. Rosanske Consulting Overland Park, KS, USA Shelley R. Rabel Riley, Department of Natural Sciences, Northwest Missouri State University, Maryville, MO, USA; Riley and Rabel Consulting Services, Maryville, MO, USA ELSEVIER AMSTERDAM • BOSTON • HEIDELBERG • LONDON • NEW YORK • OXFORD PARIS • SAN DIEGO • SAN FRANCISCO • SYDNEY • TOKYO Contents lisl Ol ('(iniiibulors PART 1 INTRQDUCT1QN CHAPTER 1 Introduction Christopher M. Riley. Bradford J. Mueller. Thomas W. Rosanske. Shelley R. Rabel Riley CHAPTER 2 General principles and regulatory considerations: specifications Christopher M. Riley. Laureen E. Little CHAPTER 3 CHAPTER 4 PART 2 \n 3 9 Application of quality by design (QbD) to the development and Validation of analytical methods David K. Lloyd. James Bergum 29 General principles and regulatory considerations: method Validation Thomas W, Rosanske, Rudlnid I. MuoMor 73 UNIVERSAL TESTS CHAPTER 5 Description and identification E.rnost Parontc CHAPTER 6 Assay and impurities Christopher M. R11ev. Shelley R. Rabri Riley. Rotiv'i l . PhHps 109 CHAPTER 7 Residual solvents James V. McArdle 143 CHAPTER 8 Validation of procedures for elemental impurities Todd L. Cer.il 155 PART 3 91 SPECIFIC TESTS: DRUG SUBSTANCE CHAPTER 9 Solid-state characterization Patrick A. Tishmark. Pmj; Chcn. P,;mHa A. Smith 173 CHAPTER 10 Chiral methods Brian He. David K. Lloyd 193 CHAPTER 11 Water determination Nilusha L.T. Padivitage. Jonathan P. Smuts, Danirl W. Armstrong 223 V vi Contents PART 4 SPECIFIC TESTS: DRUG PRODUCT CHAPTER 12 Dissolution Vivian A. Gray, Thomas W. Rosanske 245 CHAPTER 13 Extractables and leachables Kurt L. Moyer, James Scull 265 PART 5 PHARMACOPEIAL METHODS CHAPTER 14 PART 6 Microbial methods Beth Ann Brescia 313 BIOLQGICAL FLUIDS CHAPTER 16 Index 293 MICROBIAL METHODS CHAPTER 15 PART 7 Pharmacopeial methods and tests Eric B. Sheinin Bioanalytical method Validation and bioanalysis in regulated settings Krzysztof Seiinger, Eliza N. Fung, Peter Bryan 325 365