Gas Phase Chromatography of Steroids

ISBN-13: 9783642867958 / Angielski / Miękka / 2012 / 384 str.

Kristen B. Eik-Nes; Evan C. Horning

Opis

Few fields have advanced faster over the past quinquennium than separation and estimation of steroids by the technique of gas phase chromatography. A detailed and complete review of this topic would therefore be beyond the scope of the authors contributing to this monograph. It was, however, felt that a discussion of some of the highlights of this rapid advance might be of help for laboratories estimating steroids in biological samples. One of the difficulties in producing a monograph of this kind is that before it can appear in print it is likely that some of the methods it discusses will have been overtaken by better methods, so swiftly is progress now made. No editorial power has been exercised in trying to make a uni form account of technology in this field, and the idiosyncrasies of each individual author have been left intact. Through this approach we hope that what has been lost in scholarly appearance is regained in general appeal."

Spis treści

1 Gas Phase Analytical Methods for the Study of Steroid Hormones and their Metabolites.- I. Historical.- II. Analytical Methods.- 1. Single Component Analyses.- a) By High-sensitivity Non-selective Detection.- b) By High-sensitivity Selective Detection.- 2. Group Analyses.- 3. Multicomponent Analyses.- III. Instrumental Components.- 1. The Column and its Packing.- a) Column Types.- b) Supports.- c) Liquid Phases.- d) Preparation of Column Parkings.- 2. Detection Systems.- a) Hydrogen Flame Ionization.- b) Electron Capture.- c) Other Systems.- 3. Sample Introduction.- a) Samples in Solution.- b) Solid Injection.- IV. Derivatives.- 1. Reactions of Hydroxyl Groups.- 2. Reactions of Keto Groups.- 3. Reactions of Acids.- 4. Steroid Hormone Derivatives.- V. Separation Methods.- 1. With Non-selective Phases.- 2. With Selective Phases.- 3. Column Efficiency.- VI. GLC Characterization of Steroids.- 1. Relative Retention Time.- 2. Methylene Unit (MU) Values.- 3. Steroid Number (SN) Values.- VII. Problems of Quantification.- 1. Precision of GLC Systems (Flame Detection).- 2. Accuracy of GLC Systems (Flame Detection).- 3. Radioassay of GLC Effluent.- VIII. Analytical Applications with High-sensitivity Selective Detection.- IX. Structural Analysis by Gas Chromatography-Mass Spectrometry.- 1. The Gas Chromatograph-Mass Spectrometer as a Combined Instrument.- 2. Structural Analytical Methods.- X. Steroid Conjugates.- 1. ?-D-Glucosiduronic Acids.- 2. Sulfates.- References.- 2 Gas Phase Chromatographic Methods for Estrogens in Biological Fluids.- I. Introduction.- II. General Considerations.- 1. Hydrolysis.- 2. Extraction.- 3. Purification.- a) Solvent Partition.- b) Column Chromatography.- c) Thin-layer Chromatography.- d) Paper Chromatography.- e) Gel Chromatography.- III. Use of Estrogen Derivatives.- 1. Girard Separation.- 2. Methyl Ethers.- 3. Acetates.- 4. Trimethylsilyl Ethers (TMSi Ethers).- 5. O-Methoximes.- 6. Acetonides.- 7. Derivatives of Estrogens for Electron Capture Detection.- a) Chloroacetates.- b) Heptafluorobutyrates.- c) Monochloroalkylsilyl Ethers.- d) Pentafluorophenylhydrazones.- IV. Quantification and Identification of Gas Chromatographic Peaks of Estrogens.- V. Methods for the Estimation of Estrogens in Biological Extracts.- 1. Methods for Estriol in Urine of Pregnant Women.- 2. Methods for the Estimation of Estrone, Estradiol-17? and Estriol in Pregnancy Urine.- 3. Methods for the Estimation of Estrone, Estradiol and Estriol in Nonpregnancy Urine.- 4. Methods for the Estimation of Estrone, Estradiol, Estriol and other Estrogens in Pregnancy Urine.- 5. Methods for the Estimation of Estrogens in Blood.- 6. Methods for the Estimation of Estrogens in Bile.- 7. Method for the Estimation of Estrogens in Tissue Extracts.- VI. Conclusion.- References.- 3 Gas Phase Chromatography of Progesterone and Related Steroids.- I. Introduction.- 1. “Metabolism” of Progesterone.- 2. Qualitative Considerations.- 3. Quantitative Considerations.- II. Progesterone and Reduced Metabolites: Progesterone, 20?- and 20?-Hydroxypregn-4-en-3-one, 3? and 3?-Hydroxypregn-4-en-3-one, and Pregn-4-ene-3,20-Diols.- 1. Qualitative Observations.- 2. Excretion in Urine.- 3. Quantitative Estimation in Blood and Tissue.- 4. Sensitivity of Detection.- 5. Methods for Estimation in Human Peripheral Blood.- 6. Measurement of Progestins in Laboratory Animals.- 7. Conclusion.- III. Pregnanolones.- IV. Pregnanediols.- 1. Gas Chromatographic Separation of Isomeric Pregnanediols.- 2. Quantitative Estimation of Pregnanediol in Human Urine.- 3. Sensitivity of Detection.- 4. Specificity.- 5. Routine Estimations of Free Pregnanediol.- 6. Routine Estimations of Pregnanediol Diacetate.- 7. Routine Estimations of Pregnanediol Trimethylsilyl Ether.- 8. Accuracy and Precision.- 9. Conclusion.- V. 17?-Hydrogyprogesterone and Reduced Metabolites.- VI. Pregnanetriol in Human Urine.- VII. 6-Oxygenated Progesterone and Reduced Metabolites.- VIII. 11-Oxygenated Progesterone and Reduced Metabolites.- IX. 16-Oxygenated Progesterone and Reduced Metabolites.- X. 17?-Pregnanes.- XI. Other Pregnanes.- References.- 4 Gas Phase Chromatography of Androgens in Biological Samples.- I. Introduction.- II. Androgens in Blood Plasma.- 1. Testosterone in Plasma.- Conclusion.- 2. ?4-Androstenedione in Plasma.- Conclusion.- 3. 17-Ketosteroids (17-KS) in Plasma.- Conclusion.- III. Androgens in Urine.- 1. Testosterone in Urine.- Conclusion.- 2. 17-Ketosteroids in Urine.- Conclusion.- References.- 5 Gas Phase Chromatography of Corticosteroids in Biological Samples.- I. Introduction.- II. Cortisol, Prednisolone and Some of Their Metabolites.- 1. Thermal Decomposition Products.- 2. Oxidation Products.- a) Extraction.- b) Thin-layer Chromatography.- c) Bismuthate Oxidation.- d) Trimethylsilyl (TMSi) Ether Formation.- e) Gas Phase Chromatography.- f) Reproducibility.- g) Accuracy.- h) Recovery.- 3. Group Assay.- 4. Derivatives.- a) Bismethylenedioxy Derivatives.- b) 17?-Carbomethoxy Derivatives.- c) Acetates.- d) Heptafluorobutyrate Derivatives.- e) O-Methyloxime or Methoxime (MO) Derivatives.- f) Trimethylsilyl Ether Derivatives.- g) O-Methyloxime-trimethylsilyl Ether Derivatives.- h) Acetonides.- III. Corticosterone and its Metabolites.- 1. Oxidation Products.- 2. Derivatives.- a) 17?-Carbomethoxy Derivatives.- b) Acetates.- c) Trimethylsilyl Ether Derivatives.- d) O-Methyloxime-trimethylsilyl Ether Derivatives.- e) Acetonides.- IV. Aldosterone.- 1. Oxidation Products.- 2. Derivatives.- a) Acetates.- b) Trimethylsilyl Ether Derivatives.- V. Conclusion.- References.- Trivial and Systematic Names of Steroids.- Author Index.- Compound Index.- Steroid Technique Index.- Steroid Assay Index.