Gas Chromatography of Steroids in Biological Fluids: Proceedings of the Workshop on Gas-Liquid Chromatography of Steroids in Biological Fluids PDF
Preview Gas Chromatography of Steroids in Biological Fluids: Proceedings of the Workshop on Gas-Liquid Chromatography of Steroids in Biological Fluids
GAS CHROMATOGRAPHY OF STEROIDS IN BIOLOGICAL FLUIDS GAS CHROMATOGRAPHY OF STEROIDS IN BIOLOGICAL FLUIDS Proceedings of the Workshop on Gas-Liquid Chromatography of Steroids in Biological Fluids Held February 25-27, 1965, at Airlie House, Warrenton, Virginia Edited by Mortimer B. lipsett, M. D. PLEN U M PRESS NEW YORK 1965 The Workshop on Gas-Liquid Chromatography of Steroids in Biological Fluids was supported by Grant AM-9l80 from the National Institute of Arthritis and Metabolic Diseases to Dr. R. M. Dodson University of Minnesota, Minneapolis, Minnesota Library of Congress Catalog Card Number 65-25243 ISBN-13: 978-1-4684-0693-1 e-ISBN-13: 978-1-4684-0691-7 DOl: 10.1007/978-1-4684-0691-7 ©1965 Plenum Press Softcover reprint oft he hardcover 1st edition 1965 A Division of Consultants Bureau Enterprises, Inc. 227 West17th St1'eel • New York, N. Y.10011 All rights reserved CONTENTS INTRODUCTION ............•...................•..••..•...... " ..•.......•....•...• ix EDITOR'S NOTE .•.....••..•.•....•..•...•..•..••....•.••..•..•....•.....•......... xi LIST OF PARTICIPANTS •••••••••••••••••••••••••••••..••••••••••••••••••••••••••••• xiii LIST OF ABBREVIATIONS •.••••••••••••••.••••..•..••••••.•••••••••••••••.••.•••..•• xv STEROIDS - TRIVIAL AND CHEMICAL NAMES •••.•..•••.••.••.•••.••••.••••••••••.•••••• xvii SESSION I: KETOSTEROIDS AND TESTOSTERONE THE SPECIFICITY OF A GAS CHROMATOGRAPHIC METHOD FOR THE DETERMINA TION OF URINARY ANDROSTERONE, ETIOCHOLANOLONE AND DEHYDROEPIANDRO STERONE IN URINE by B. S. Thomas................................................. 1 THE INDIRECT ANALYSIS OF URINARY l7-0XYGENATED C19 STEROID SULPHATES BY GAS-LIQUID CHROMATOGRAPHY by E. Menini.................................................... 11 A TECHNIC FOR FRACTIONATION OF l7-KETOSTEROIDS FROM URINE by C. R. Berrett and C. McNeiL................................. 17 GAS CHROMATOGRAPHIC METHOD FOR THE DETERMINATION OF TESTOSTERONE IN HUMAN URINE by W. Futterweit, G. L. Siegel, R. Freeman, S. I. Griboff, M. Drosdowsky, N. Gibree, R. 1. Dorfman and L. J. Soffer........ 19 ESTIMATION OF TESTOSTERONE IN BLOOD BY GAS-LIQUID CHROMATOGRAPHY by A. C. Brownie................................................ 23 THE ESTIMATION OF PLASMA ANDROGENS BY GAS-LIQUID CHROMATOGRAPHY by A. Goldfien, J. Jones, M. E. Yannone and B. White............ 35 DISCUSSION.......................................................... 43 SESSION II: CORTICOIDS THE ESTIMATION OF UNCONJUGATED CORTISOL METABOLITES IN URINE BY GAS CHROMATOGRAPHY by E. Bailey.................................................... 57 GAS CHROMATOGRAPHY OF CORTOLS AND CORTOLONES by R. S. Rosenfeld.............................................. 67 v URINARY CORTICOIDS BY GAS CHROMATOGRAPHY by M. G. Crane and J. J. Harris................................ 73 A SPECIFIC METHOD FOR THE GAS CHROMATOGRAPHIC DETERMINATION OF ALDOSTERONE AND ADRENOCORTICAL STEROIDS: APPLICATION TO ADRENAL VENOUS BLOOD OF VERTEBRATES by H. Gottfried................................................ 89 ANALYSIS OF ALDOSTERONE IN URINE BY DOUBLE ISOTOPE DILUTION AND GAS-LIQUID CHROMATOGRAPHY by B. Kliman................................................... 101 DISCUSSION......................................................... 113 SESSION III: PROGESTERONE AND C21-DIOLS AND TRIOLS MEASUREMENT OF URINARY STEROIDS BY GAS CHROMATOGRAPHY. 3G',17- DIHYDROXYPREGNANE-20-0NE AND C21 TRIOLS by R. S. Rosenfeld ••••••••••••••••••••••••••••• 127 0 • • • • • • • • • • • • • • • ANALYSIS OF URINARY PREGNANEDIOL AND PREGNANETRIOL BY GAS-LIQUID CHROMATOGRAPHY by M. A. Kirschner and M. B. Lipsett ••••••••••••••••••••••••••• 135 THE APPLICATION OF GAS-LIQUID CHROMATOGRAPHY TO THE MEASUREMENT OF PLASMA PROGESTERONE by A. Goldfien, M. E. Yannone, D. B. McComas and C. Braga •.•••. 143 DETERMINATION OF PROGESTERONE IN HUMAN PERIPHERAL BLOOD USING GAS-LIQUID CHROMATOGRAPHY WITH ELECTRON CAPTURE DETECTION by H. J. van der Molen and D. Groen............................ 153 THE ANALYSIS OF PLASMA PROGESTINS BY GAS CHROMATOGRAPHY by I. H. Carlson, A. J. Blair and R. K. Meyer •.•••..••••..••••• 169 DISCUSSION......................................................... 177 SESSION IV: ESTROGENS GAS CHROMATOGRAPHY AND ITS ROLE IN THE VERSATILE ANALYSIS OF URINARY ESTROGENS by H. H. Wotiz and S. C. Chattoraj ••••••••••••••••••••••••••••• 195 DETERMINATION OF URINARY ESTROGENS BY GAS CHROMATOGRAPHY by H. Adlercreutz and T. Luukkainen ••.••••••.••..•.•••.•••••••• 215 GAS CHROMATOGRAPHY OF ESTRIOL IN PREGNANCY URINE by J. C. Touchstone............................................ 229 ANALYSIS OF ESTROGENS IN THE URINE OF NON-PREGNANT WOMEN BY GAS LIQUID CHROMATOGRAPHY by E. Menini................................................... 233 vi THE MEASUREMENT OF ESTRIOL IN URINE AND AMNIOTIC FLUID BY GAS-LIQUID CHROMATOGRAPHY by A. E. Schindler, M. C. Lindberg and W. L. Herrmann •••.••••.• 237 GAS CHROMATOGRAPHY OF FREE AND CONJUGATED ESTROGENS IN BLOOD PLASMA by J. C. Touchs tone and T. Murawec............................. 243 ESTIMATION OF ESTRADIOL-17~ BY GAS-LIQUID CHROMATOGRAPHY WITH ELECTRON CAPTURE DETECTION by K. B. Eik-Nes, A. Aakvaag and L. J. Grota •••.••••••••..••••• 247 GAS CHROMATOGRAPHY OF ESTROGENS AND OTHER STEROIDS FROM ENDOCRINE TISSUES by K. W. McKerns and E. Nordstrand ••••••••••••••••••••••••••••• 255 DISCUSSION......................................................... 263 SESSION V: SOME THEORETICAL AND PRACTICAL ASPECTS OF GAS-LIQUID CHROMATOGRAPHY SOME ASPECTS OF THE CHEMISTRY OF GAS-LIQUID CHROMATOGRAPHY by W. J. A. VandenHeuvel....................................... 277 DISCUSSION......................................................... 292 SOME PRACTICAL PROBLEMS IN GAS-LIQUID CHROMATOGRAPHY by H. M. Fales................................................. 297 COMMENTS ON TECHNIQUES ON GAS CHROMATOGRAPHY by H. H. Wotiz................................................. 301 DISCUSSION. •• . • • • • • • • • • • • • • • • •• • • • • • • • • • • • • • • • • . • • • • • • • • • • • • • . • • • • • 307 THE UTILITY OF GLC FOR ANALYZING SPECIFIC STEROIDS IN BIOLOGICAL FLUIDS by A. Karmen................................................... 309 INDEX........................................................................... 313 vii INTRODUCTION During the past decade we have witnessed a revolution in analytical methods. The development of vapor phase chromatography for the separation and analysis of classes of substances ranging from metals and gases to a wide variety of organic materials has been one of the most exciting of these new techniques. Gas-liquid chromatography for the measurement of steroids is particularly significant for endocrinologists and reports during the past several years have demonstrated its usefulness. Because of the growing interest in this method, a committee of the Endocrinology Study Section composed of Drs. R. M. Dodson, Seymour Lieberman, Hilton A. Salhanick, and Ralph E. Peterson, felt that the time was propitious to hold this Workshop and it is on their behalf that I welcome you. We hope to obtain enough data during these sessions so that those attending this conference and those who may read the proceedings will be able to make an informed judgement about the usefulness of gas-liquid chromatography for the analysis of steroids in biological fluids. Thus, I hope that there will be adequate documentation of the reliability of the methods as well as a comparison of the advantages and disadvantages of this analytical method with other classical methods. If we can do this, this Workshop will provide a significant base of practical considerations about gas chromatographic analytic techniques. I would like to thank Drs. T. F. Gallagher, H. Wilson, H. Salhanick and L. Engel for agreeing to serve as Chairmen of the sessions. ix EDITOR'S NOTE This book is divided into five sections: gas-liquid chromatography of ketosteroids, corti coids, estrogens, progestins, and some practical considerations in gas chromatography. Discussion follows each section. A list of abbreviations and of trivial names and abbreviations for steroids has been provided. An attempt has been made to index the discussion material and pertinent ele ments in the papers. A word of caution seems appropriate here. Of the participants at this Workshop, only a few can be classified as professionals in the area of gas chromatography. The others are biologists or physicians who have attempted to use this technique with varying degrees of success. This book therefore is not a repository of wisdom about gas chromatography but is probably instead a fair reflection of the practice of the art as of 1965. Many of these methods will be revised, improved, or abandoned in the future and it is almost certain that none can be considered definitive at pre sent. However, some of these methods have proved useful already and are worthy of consideration. Caveat emptor! xi LIST OF PARTICIPANTS Bailey, E., Sheffield, England Brownie, A. C., Buffalo, New York Carlson, I. H., Madison, Wisconsin Crane, M. G., Lorna Linda, California Dodson, R. M., Minneapolis, Minnesota Eik-Nes, K. B., Salt Lake City, Utah Engel, L., Boston, Massachusetts Fales, H. M., Bethesda, Maryland Futterweit, W., New York City Gallagher, T. F., New York City Goldfien, A., San Francisco, California Gottfried, H., Sheffield, England Karmen, A., Baltimore, Maryland Kirschner, M. A., New York City Kliman, B., Boston, Massachusetts Lieberman, S., New York City Lipsett, M. B., Bethesda, Maryland Luukkainen, T., Helsinki, Finland McKerns, K. W., Gainesville, Florida McNeil, C., Salt Lake City, Utah Menini, E., Edinburgh, Scotland Patti, A., Philadelphia, Pennsylvania Rosenfeld, R. S., New York City Salhanick, H., Boston, Massachusetts Schindler, A. E., Seattle, Washington Thomas, B. S., London, England Touchstone, J. C., Philadelphia, Pennsylvania VandenHeuvel, W. J. A., Rahway, New Jersey van der Molen, H. J., Utrecht, The Netherlands Wilson, H., Bethesda, Maryland Wotiz, H. H., Boston, Massachusetts xiii LIST OF ABBREVIATIONS Centigrade C Centimeter (s) cm Counts per minute cpm Disintegrations per minute dpm Gas-liquid chromatography (ic) GLC Gram (s) g Hour (s) hr Inside diameter id Kilogram kg Meter m Microgram ~g Microliter ~l Microsecond (s) ~sec Milligram mg Millimicrogram Minute (s) min Normal (concentration) N Outside diameter od Pounds per square inch psi Relative retention time R t Retention time RT Specific activity SA 2 Square centimeters cm Standard deviation SD Standard error SE Thin-layer chromatography (ic) TLC Trimethylsilyl TMS Volume (s) vol xv
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