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Modern Methods of Steroid Analysis


Author: Erich Heftmann

Publisher: Academic Press

Publish Date: 1st January 1973

ISBN-13: 9780323146449

Pages: 544

Language: English



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