Ahuja / Jimidar Capillary Electrophoresis Methods for Pharmaceutical Analysis

1. Auflage 2011
ISBN: 978-0-08-055961-2
Verlag: Elsevier Science & Techn.
Format: PDF
Kopierschutz: 1 - PDF Watermark

E-Book, Englisch, 546 Seiten, Web PDF

Capillary electrophoresis (CE) is a powerful analytical technique that is widely used in research and development and in quality control of pharmaceuticals. Many reports of highly efficient separations and methods have been published over the past 15 years. CE offers several advantages over high-pressure or high-performance liquid chromatography (HPLC). These include simplicity, rapid analysis, automation, ruggedness, different mechanisms for selectivity, and low cost. Moreover, EC requires smaller sample size and yet offers higher efficiency and thus greater resolution power over HPLC. These characteristics are very attractive in research and development, even more so in pharmaceutical quality control (QC) and stability monitoring (SM) studies. This book will provide busy pharmaceutical scientists a complete yet concise reference guide for utilizing the versatility of CE in new drug development and quality control.
- Provides current status and future developments in CE analysis of pharmaceuticals.
- Explains how to develop and validate methods.
- Includes major pharmaceutical applications including assays and impurity testing.

Autoren/Hrsg.

Ahuja, Satinder

Jimidar, Mohamedilias

Inhaltsverzeichnis

1;Front cover;1
2;Capillary Electrophoresis methods for Pharmaceutical analysis;4
3;Copyright page;5
4;Contents;6
5;Preface;14
6;Contributors;16
7;Chapter 1. Overview of capillary electrophoresis in pharmaceutical analysis;18
7.1;I. Introduction;18
7.2;II. Various modes of CE;19
7.3;III. Instrumentation;20
7.4;IV. Method development for pharmaceutical analysis;20
7.5;V. Analysis of active pharmaceutical ingredients and drug products;20
7.6;VI. General considerations for improving performance of CE methods;21
7.7;VII. Current regulatory guidance;21
7.8;VIII. Qualification of capillary electrophoresis instrumentation;21
7.9;IX. Robustness tests of CE methods;22
7.10;X. Validation of analytical methods;22
7.11;XI. The need for CE methods in pharmacopoeias;22
7.12;XII. CE in impurity profiling of drugs;23
7.13;XIII. Ion analysis using capillary electrophoresis;23
7.14;XIV. Role of CE in biopharmaceutical development and QC;23
7.15;XV. Capillary electrophoresis and bioanalysis;24
7.16;XVI. CE as an orthogonal technique to chromatography;24
7.17;XVII. Capillary electrochromatography of pharmaceuticals;24
7.18;XVIII. Coupling CE and microchip-based devices with mass spectrometry;24
7.19;References;25
8;Chapter 2. Theoretical considerations in performance of various modes of CE;26
8.1;I. Introduction;27
8.2;II. Basic CE configuration;28
8.3;III. CE characteristics;29
8.4;IV. Principles of CE;34
8.5;V. Methods and modes in CE;48
8.6;VI. Summary and conclusions;56
8.7;References;57
9;Chapter 3. Equipment considerations for capillary electrophoresis;60
9.1;I. Capillary electrophoresis instrumentation;61
9.2;II. Equipment-related issues;73
9.3;III. Validation and compliance requirements;74
9.4;IV. Future developments;76
9.5;V. Summary;78
9.6;References;78
10;Chapter 4. Method development for pharmaceutical analysis;80
10.1;I. Introduction;81
10.2;II. CE method types used in QC testing;84
10.3;III. Method development process;86
10.4;IV. Planning phase;87
10.5;V. Method development and optimization;91
10.6;VI. System suitability tests and limits;98
10.7;VII. Draft method description and method evaluation phase;107
10.8;VIII. Method validation phase;108
10.9;IX. Method transfer phase;108
10.10;X. Method performance monitoring and feedback;110
10.11;XI. Summary and conclusions;111
10.12;References;111
11;Chapter 5. Role of CE in drug substance and drug product development;112
11.1;I. Introduction;113
11.2;II. When should CE be applied in drug development?;116
11.3;III. Capillary electrophoresis in the drug development process, from candidate selection to the market;119
11.4;IV. Pharmaceutical substances in literature;136
11.5;V. Summary and conclusions;136
11.6;References;137
12;Chapter 6. General considerations to improve performance of CE methods;140
12.1;I. Introduction;141
12.2;II. Capillary;142
12.3;III. Electrodes;144
12.4;IV. Temperature;145
12.5;V. Preconditioning;145
12.6;VI. Injection;147
12.7;VII. Applied voltage;149
12.8;VIII. Background Electrolyte;150
12.9;IX. Detection and Signal Integration;155
12.10;X. Summary and conclusions;157
12.11;Acknowledgements;157
12.12;References;158
13;Chapter 7. Overview of current regulatory guidance;162
13.1;I. Introduction;163
13.2;II. Regulatory guidance documents;163
13.3;III. Capillary electrophoresis in pharmacopoeias;168
13.4;IV. Conclusions;181
13.5;References;182
14;Chapter 8. Qualification of CE instrumentation;188
14.1;I. Introduction;189
14.2;II. Parameters for Qualification;191
14.3;III. Computer System;192
14.4;IV. Keeping the Instrument qualified;200
14.5;References;200
15;Chapter 9. Robustness testing of CE methods;202
15.1;I. Introduction;203
15.2;II. Aims/objectives and steps in a robustness test;204
15.3;III. Selection of factors and levels;206
15.4;IV. Selection of experimental designs;211
15.5;V. Selection of responses;215
15.6;VI. Planning and execution of experimental work;217
15.7;VII. Analysis of results;219
15.8;VIII. Determination of SST limits;219
15.9;IX. Review of case studies;227
15.10;X. Summary and conclusions;236
15.11;References;237
16;Chapter 10. Validation of analytical methods using capillary electrophoresis;242
16.1;I. Method validation;243
16.2;II. Instrument qualification;257
16.3;III. Method transfer;259
16.4;IV. Summary;260
16.5;Abbreviations;260
16.6;References;261
17;Chapter 11. The need for CE methods in pharmacopoeial monographs;262
17.1;I. Introduction;262
17.2;II. Key factor for the development of a robust CE method and validation;264
17.3;III. Overcoming the problem of low sensitivity;265
17.4;IV. Methods in the European pharmacopoeia;266
17.5;V. Chiral analysis;271
17.6;VI. Conclusions;273
17.7;Acknowledgements;273
17.8;References;273
18;Chapter 12. CE in impurity profiling of drugs;276
18.1;I. Introduction;277
18.2;II. Overview of CE applications in impurity profiling;278
18.3;III. Concluding remarks;316
18.4;References;316
19;Chapter 13. Ion analysis using capillary electrophoresis;334
19.1;I. Introduction;335
19.2;II. General principle;336
19.3;III. Method development and optimization;350
19.4;IV. Applications;356
19.5;Case Study I. Example of counterion determination;356
19.6;Case Study II. Example of a feasibility study for impurity profiling;365
19.7;V. Conclusions;368
19.8;References;368
20;Chapter 14. Role of CE in biopharmaceutical development and quality control;374
20.1;I. Introduction;375
20.2;II. Method development and qualification;375
20.3;III. Method transfer;407
20.4;IV. Method performance in QC environment;408
20.5;V. Lessons learned;409
20.6;VI. Conclusions;410
20.7;Acknowledgments;410
20.8;Appendix. Troubleshooting examples;410
20.9;References;416
21;Chapter 15. Capillary electrophoresis and bioanalysis;418
21.1;I. Introduction;419
21.2;II. Capillary electrophoresis sodium dodecyl sulfate (CE-SDS);419
21.3;III. Effect of sample preparation on CE-SDS and SDS-PAGE analysis of rMAbs;423
21.4;IV. Capillary zone electrophoresis;429
21.5;V. Capillary isoelectric focusing;430
21.6;VI. Carbohydrate analysis by CE-LIF;434
21.7;VII. CE and quality control testing of therapeutic proteins;435
21.8;VIII. Conclusions;439
21.9;Acknowledgments;440
21.10;References;440
22;Chapter 16. CE as an orthogonal technique to chromatography;442
22.1;I. Introduction;443
22.2;II. Orthogonal chromatographic systems;444
22.3;III. CE as an orthogonal technique;450
22.4;IV. Conclusions;452
22.5;References;452
23;Chapter 17. Capillary electrochromatography of pharmaceuticals;456
23.1;I. Introduction;457
23.2;II. Factors affecting the electrophoretic and chromatographic parameters in CEC;459
23.3;III. Column technology in CEC;467
23.4;IV. Types of columns used in CEC;468
23.5;V. Analyte detection in CEC;475
23.6;VI. Applications of capillary electrochromatography;478
23.7;VII. Two-dimensional separations;484
23.8;VIII. Validating CEC methods for pharmaceutical analysis;486
23.9;IX. CEC-prospects and potentials;487
23.10;References;488
24;Chapter 18. Coupling CE and microchip-based devices with mass spectrometry;494
24.1;I. Introduction;495
24.2;II. CE-MS coupling and instrumentation;496
24.3;III. Applications;502
24.4;IV. Quantitative Aspects;510
24.5;V. New devices;512
24.6;VI. Summary and conclusions;517
24.7;Abbreviations;517
24.8;References;519
25;Index;540