Vol 1 1997.pdf

HPLC METHODS

FOR PHARMACEUTICAL

ANALYSIS

George Lunn and Norman R. Schmuff

A WILEY-INTERSCIENCE PUBLICATION

JOHN WILEY & SONS, INC.

New York / Chichester / Weinheim / Brisbane / Singapore / Toronto

This text is printed on acid-free paper.

Reproduction or translation of any part of this work beyond

that permitted by Section 107 or 108 of the 1976 United

States Copyright Act without the permission of the copyright

owner is unlawful. Requests for permission or further

information should be addressed to the Permissions Department,

John Wiley & Sons, Inc., 605 Third Avenue, New York, NY

10158-0012.

Library of Congress Cataloging in Publication Data:

Lunn, George.

HPLC methods for pharmaceutical analysis / by George Lunn and

Norman R. Schmuff.

p. cm.

Includes bibliographical references and index.

ISBN 0-471-18176-5 (cloth : alk. paper)

1. High performance liquid chromatography. 2. Drugs—analysis.

I. Schmuff, Norman R. IL Title.

[DNLM: 1. Drugs—analysis. 2. Chromatography, High Pressure

Liquid—methods. 3. Chemistry, Pharmaceutical—methods. QV 25

L936h 1996]

RS189.5.H54L77 1996

615M901—dc20

DNLM/DLC

for Library of Congress

96-29417

CIP

ISBN 0-471-18176-5 (Book only)

ISBN 0-471-18198-6 (CD-ROM only)

ISBN 0-471-13078-8 (Book/CD-ROM set)

Printed in the United States of America

10 9 8 7 6 5

PREFACE

This book is a collection of procedures for the analysis of a number of pharmaceu-

ticals using high-performance liquid chromatography (HPLC). For each compound

various techniques are described in sufficient detail that the analyst can replicate

the procedure without reference to the original publication. Since detailed proce-

dures for the same drug are listed together, it is very easy for the researcher to

combine features of different methods, e.g., the extraction procedure from one paper

and the chromatographic procedure from another paper, to provide methods tai-

lored to the researcher's requirements. In addition to the detailed procedures, bib-

liographies are provided listing other references. These references are annotated

so that the reader can rapidly determine those procedures likely to be of the most

utility. In the current volume, we have listed procedures for the analysis of the

most commonly used drugs in the United States. 1 ' 2 In future volumes we hope to

cover the remaining drugs used for medical and veterinary purposes.

The impetus for writing this book was the realization that there was no single

volume listing analytical procedures and that there was, in particular, no ready

source of information on the analysis of drugs in biological fluids other than the

original literature. Although a number of methods are in common use for the anal-

ysis of Pharmaceuticals, HPLC may be regarded as the "gold standard" 3 and so we

have decided to concentrate on this procedure. For example, HPLC assays of an-

tibiotics have advantages such as specificity, better accuracy and precision, and

wider availability of equipment, over other methods. Thus, HPLC procedures are

gradually coming to replace other techniques. 4

Although the universal penetration of computers has led to readily available

laboratory-based searches of the literature, this resource is not exploited as much

as it might be. An FDA inspector has stated 5 that many pharmaceutical firms, when

questioned about deficiencies in this area, admit to never having performed a lit-

erature search for HPLC methods. One reason for this reluctance is, of course, that

a computer search merely produces a listing of possibly relevant references. Tedious

and time-consuming searches in the library are necessary to find the most relevant

reference that can be turned into a practical analytical procedure in the searcher's

own laboratory. The reference finally chosen will depend on the individual circum-

stances such as the matrix in which the drug is present and availability of equip-

ment. This book circumvents this lengthy process by providing a number of ab-

stracted and evaluated procedures for the analysis of each drug. The analyst can

rapidly identify a relevant procedure and put it into practice without having to

consult the original literature. For many compounds the number of analytical pro-

cedures is so large that it is not possible to fully abstract all of them. For this

reason we have added annotated bibliographies so that the researcher can rapidly

identify a relevant paper without having to locate and evaluate a large number of

irrelevant procedures.

In addition to the analytical matrix, other factors may be important when choos-

ing an analytical procedure. Accordingly, we have noted other features of analytical

procedures such as sensitivity, mode of detection, other compounds that interfere

with the analysis, and other drugs that may be determined at the same time.

We would like to thank the staff of the NCI-Frederick Cancer Research and

Development Center Scientific Library for their help with this project. In particular,

we would like to thank Pat Kuhns-Kelly for her diligent assistance with the com-

puter searches and Ethel Armstrong for her indefatigable efforts in obtaining many

of the more obscure references via Interlibrary Loan. The use of the NIH Library,

National Institutes of Health, Bethesda, MD, is also greatly appreciated. We would

also like to thank Perry King of John Wiley for help with the electronic version.

Special thanks are due to our editor, Betty Sun, who brought the whole project

together. The initial research which later became the nucleus of this book was

supported by the Division of Safety, NIH, through NCI contract NO1-CO-74102

with Program Resources, Inc. Although many people have helped with the prepa-

ration of this work, the mistakes are our own. We would appreciate hearing from

anyone who has corrections, comments, or suggestions. We can be reached at

71061.2731@compuserve.com or norman.schmuff@tcs.wap.org.

The content of this publication does not necessarily reflect the views, policies, or

guidelines of the Department of Health and Human Services or the Food and Drug

Administration, nor does mention of trade names, commercial products, or organ-

izations imply endorsement by the U.S. Government.

REFERENCES

1. American Druggist 1993, 207(3), 49-53.

2. Med Ad News, 1995 (May), 22.

3. Jones, P.M.; Brune, K. Monitoring cyclosporine by HPLC with cyclosporin C as internal

standard. CUn. Chem. 1993, 39, 168-169.

4. Wright, W.W. Use of liquid chromatography for the assay of antibiotics. Pharmacopeial

Forum 1994, 20, 8155-8159.

5. Roos, R.W. Validation issues in high pressure liquid chromatographic methods for phar-

maceuticals. Abstract #15, 27th Middle Atlantic Regional Meeting of the American Chem-

ical Society, Hempstead, NY, June 2-4, 1993.

ABOUT THIS BOOK

SCOPE

Based on surveys of the top 200 drugs by number of prescriptions filled 1 and the

top 100 drugs by dollar sales, 2 we selected the most commonly used drugs in the

United States. Analytical procedures for these drugs are described in this book. In

future volumes, we hope to cover other drugs used for medical and veterinary

purposes.

After the target compounds were identified, a computer search was used to iden-

tify relevant references. In general, the computer search was conducted using Med-

line, 1980 to 1996, but for a few of the most common drugs the complete Chemical

Abstracts file on Dialog was used. Tests showed that retrieval using Dialog and

Medline was similar, except that references from the Journal of Liquid Chroma-

tography are not included in Medline. All relevant references from the Journal of

Liquid Chromatography (1980 to 1996) were manually added to the database.

In Medline the search strategy was:

HPLC (tw) or HPLC (mh) or liquid chromatography (mh)

and USAN drug name (tw or mh) where tw = text word and mh = MESH heading.

In addition to the Medline search some journals were routinely surveyed for

relevant articles. These journals were:

American Journal of Health-System Pharmacy (formerly American Journal of

Hospital Pharmacy)

Analyst

Analytical Chemistry

Antimicrobial Agents and Chemotherapy

Arzneimittelforschung

Biochemical Pharmacology

Biological and Pharmaceutical Bulletin

Biomedical Chromatography

Biopharmaceutics and Drug Disposition

Chemical and Pharmaceutical Bulletin

Chromatographia

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