Modern Methods of Steroid Analysis - 1st Edition - ISBN: 9780123366405, 9780323146449

Modern Methods of Steroid Analysis

1st Edition

Editors: Erich Heftmann
eBook ISBN: 9780323146449
Imprint: Academic Press
Published Date: 1st January 1973
Page Count: 544
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Modern Methods of Steroid Analysis reviews modern methods of steroid analysis such as liquid column chromatography, mass spectrometry, and gas chromatography. Topics covered include qualitative and quantitative analysis of plant sterols by gas-liquid chromatography; Raman spectroscopy of steroids; nuclear magnetic resonance; and applications of lanthanide shift reagents. A computerized method for rapid comparison and retrieval of infrared spectral data is also described. This volume is comprised of 22 chapters and begins with an analysis of hormonal steroids using liquid column chromatography, followed by a discussion on the separation of insect molting hormones using high-pressure liquid chromatography. The reader is methodically introduced to the application of gradient elution and thin-layer chromatography to the analysis of corticosteroids and 17-ketosteroids, as well as some aspects of mass spectrometry in steroid analysis. Subsequent chapters explore other methods such as optical rotatory dispersion and circular dichroism, along with radioisotope techniques. In particular, the radioimmunoassay of plasma steroid hormones and plasma aldosterone is considered. This book should be of interest to biochemists.

Table of Contents

List of Contributors


List of Abbreviations

Section I. Chromatography

Chapter 1. Liquid Column Chromatography of Hormonal Steroids

I. Introduction

II. Recent Developments in High-Resolution Liquid Chromatography

III. New Active-Shell/Inert-Core Materials for High-Resolution Chromatography

IV. Liquid Chromatographs

V. Application of High-Resolution, High-Speed Liquid Chromatography to Steroid Analysis

VI. Application of High-Resolution, Moderate-Speed Liquid Chromatography to Steroid Analysis

VII. Other High-Resolution, Moderate-Speed Methods for Liquid Chromatography of Steroids

VIII. Low-Resolution Liquid Chromatography of Steroids

IX. Comparison of Liquid Chromatography with Other Chromatographic Methods for Steroids

X. Conclusions


Chapter 2. Application of High-Pressure Liquid Chromatography to the Separation of Insect Molting Hormones

I. Introduction

II. Chromatographic Theory

III. Apparatus

IV. Liquid-Chromatographic Separation of Ecdysones


Chapter 3. Gradient Elution and Thin-Layer Chromatography in the Analysis of Corticosteroids and 17-Ketosteroids

I. Gradient Elution

II. Computerized Comparison of Thin-Layer Chromatograms


Chapter 4. Gas Chromatography of Steroid Hormones

I. Instrumentation

II. Steroid Derivatives

III. Structure and Chromatographic Behavior

IV. Column Selection

V. Quantitative Analysis

VI. Methodology


Chapter 5. Qualitative and Quantitative Analysis of Plant Sterols by Gas-Liquid Chromatography

I. Introduction

II. Separation Techniques

III. Gas-Liquid Chromatography

IV. Results

V. GLC of Other Sterol Types


Section II. Mass Spectrometry

Chapter 6. Some Aspects of Mass Spectrometry in Steroid Analysis

I. Introduction

II. Hydrocarbons

III. Monooxygenated Steroids

IV. Steroids Containing More than One Oxygen Group

V. Derivatives Suitable for Gas Chromatography-Mass Spectrometry

VI. Quantitative Aspects of Mass Spectrometry in Steroid Analysis

VII. Miscellaneous Steroids

VIII. Conclusions


Chapter 7. Derivatization and Gas Chromatography in the Mass Spectrometry of Steroids

I. Introduction

II. Derivatization and Characterization Techniques

III. Selective Detection by Mass Spectrometry

IV. Possible Pitfalls


Section III. Infrared and Raman Spectroscopy

Chapter 8. A Computerized Method for Rapid Comparison and Retrieval of Infrared Spectral Data

I. Introduction

II. The IRIS System

III. Use of the Information System


Chapter 9. Raman Spectroscopy of Steroids

I. Introduction

II. Preparation of the Samples

III. Characteristic Bonds in the Raman Spectra

IV. Scheme for Steroid Structure Elucidation


Section IV. Nuclear Magnetic Resonance

Chapter 10. Introduction to Nuclear Magnetic Resonance

I. Introduction

II. Nuclear Magnetic Resonance

III. The Basic NMR Spectrometer

IV. Relaxation Times and Relaxation Mechanisms

V. General Features of NMR

VI. Comparison of H and 13C NMR for Steroid Structural Studies

VII. Sensitivity of NMR Methods


Chapter 11. Applications of Lanthanide Shift Reagents

I. Introduction

II. Magnetic Interactions

III. Chemistry of Shift Reagents

IV. Applications

V. New Lanthanide Shift Reagents


Section V. X-Ray Diffraction Analysis

Chapter 12. X-Ray Analysis of Steroid Structures and the Automated Diffractometer

I. Introduction

II. General Features of the Steroid Nucleus

III. Steroid Structures of Biochemical Interest

IV. The Automated Diffractometer


Chapter 13. Application of Direct Methods of X-Ray Structure Analysis to Steroids

I. Introduction

II. Phase Relations

III. Procedure for Phase Determination

IV. An Example

V. Steroid Structures

VI. Concluding Remarks


Chapter 14. The Faltmolekül Method and Other Patterson Search Techniques in Structure Analysis

I. Introduction

II. Patterson Function

III. Faltmolekül Method

IV. Calculation

V. Application of the Faltmolekül Method to the Structure Analysis of Steroids


Section VI. Optical Rotatory Dispersion and Circular Dichroism

Chapter 15. Recent Optical Rotatory Dispersion and Circular Dichroism Studies in the Steroid Field

I. Introduction

II. Structure and Configuration

III. Ketals and Saturated Ketones

IV. Relative Configuration and Conformation

V. Absolute Stereochemistry

VI. Conjugated Cyclopropanes

VII. Dimedonyl Derivative of Amines

VIII. Cyclopropenones

IX. The Allene Chromophore


Chapter 16. Cotton Effects and Allylic-Homoallylic Chirality of Steroidal Olefins and Conjugated Dienes and Enones

I. Introduction

II. Monoenes

III. Conjugated Dienes and Trienes

IV. Conjugated Enones and Dienones

V. Other π-Bond Chromophores

VI. Conclusion


Chapter 17. Cotton Effects of Acid Derivatives, Aromatic Steroids, and Nitrogen-, Sulfur-, and Halogen-Containing Steroids

I. Carboxylic Acid Derivatives

II. Derivatives of Alcohols

III. Aromatic Steroids

IV. Nitrogen-Containing Chromophores

V. Sulfur-Containing Chromophores

VI. Steroidal Iodides


Section VII. Radioisotope Methods

Chapter 18. Estrogen Analysis by the Double Isotope Derivative Method

I. Introduction

II. Specific Activity Determination

III. Estrogen Production Rates

IV. Estrogen Excretion Rates


Chapter 19. Corticosteroid Analysis by Competitive Protein Binding

I. Introduction

II. Plasma Cortisol

III. Urinary Cortisol

IV. 11-Deoxycortisol


Chapter 20. Enzymic Isotope Displacement Assay of Digitalis Glycosides

I. Introduction

II. The Enzymic Isotope Displacement Assay

III. Results

IV. Comparison of Various Assays

V. Assay of Unknown Glycosides

VI. Relationship of Serum Digoxin Levels to Digoxin Dosage Regimens


Chapter 21. Radioimmunoassay of Plasma Steroid Hormones

I. Introduction

II. Chromatographic Separation of Steroid Hormones

III. Radioimmunoassay of Steroid Hormones

IV. Determination of Steroid Hormones in Biological Fluids

V. Future Trends


Chapter 22. Radioimmunoassay of Plasma Aldosterone

I. Introduction

II. Methods

III. Immunoassay

IV. Results and Discussion

V. Other Approaches to the Radioimmunoassay of Plasma Aldosterone


Author Index

Subject Index


No. of pages:
© Academic Press 1973
Academic Press
eBook ISBN:

About the Editor

Erich Heftmann

Affiliations and Expertise

Western Regional Research Center, United States Department of Agriculture

Ratings and Reviews