Modern Methods of Steroid Analysis

Modern Methods of Steroid Analysis

1st Edition - January 1, 1973

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  • Editor: Erich Heftmann
  • eBook ISBN: 9780323146449

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Description

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

    Preface

    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

    References

    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

    References

    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

    References

    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

    References

    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

    References

    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

    References

    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

    References

    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

    References

    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

    References

    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

    References

    Chapter 11. Applications of Lanthanide Shift Reagents

    I. Introduction

    II. Magnetic Interactions

    III. Chemistry of Shift Reagents

    IV. Applications

    V. New Lanthanide Shift Reagents

    References

    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

    References

    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

    References

    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

    References

    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

    References

    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

    References

    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

    References

    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

    References

    Chapter 19. Corticosteroid Analysis by Competitive Protein Binding

    I. Introduction

    II. Plasma Cortisol

    III. Urinary Cortisol

    IV. 11-Deoxycortisol

    References

    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

    References

    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

    References

    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

    References

    Author Index

    Subject Index

Product details

  • No. of pages: 544
  • Language: English
  • Copyright: © Academic Press 1973
  • Published: January 1, 1973
  • Imprint: Academic Press
  • eBook ISBN: 9780323146449

About the Editor

Erich Heftmann

Affiliations and Expertise

Western Regional Research Center, United States Department of Agriculture

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