Capillary Liquid Chromatography

ISBN-13: 9781468416640 / Angielski / Miękka / 2012 / 262 str.

B. G. Belen'kii; E. S. Gankina; V. G. Mal'tsev

Opis

In the early 1980s capillary liquid chromatography was being established; it was a period in which only a few research groups published a relatively small number of papers on the subject. In- terest has since taken off, and a period of intense development, to which no end is yet in sight, is now upon us. More investiga- tors and instrument-making firms are now entering the field. This greater interest has resulted in the rapid appearance of two collec- tions 1, 2] and a series of topical reviews 3-6]. However, it could hardly be said that all the problems in this area have been formulated, let alone solved. The preparation of very efficient - open tubular or packed - microbore columns, for example, remains more an art than a science, while the relation- ship between radial and longitudinal mass transfer, and the effect of transcolumn velocity profiles on chromatographic efficiency, have been very poorly studied. Indeed, recent publications on these subjects have sometimes, far from clarifying matters, only muddied them further. Many instrument-making firms are trying to unify their equip- ment so that it is suitable for microbore, conventional (analytical), and preparative liquid chromatography. This approach has not real- ized the full potential of capillary chromatography, and there also remains room for improving the performance of capillary columns.

Spis treści

1. Introduction.- 2. Development and Achievements of Capillary Liquid Chromatography.- 3. Theoretical Basis of Capillary liquid Chromatography.- 3.1. Band Spreading in Packed and Open Tubular Columns.- 3.2. Optimizing Liquid Chromatography.- 3.3. Extracolumn Spreading and Optimizing the Chromatographic System.- 3.3.1. Dispersion in the Injector Cell.- 3.3.2. Sample Mass.- 3.3.3. Dispersion in the Detector Cell.- 3.3.4. Dispersion in the Connecting Capillaries.- 3.3.5. Detector System’s Time Constant.- 3.4. Optimization with Respect to Analysis Speed.- 3.5. Optimization with Respect to Sensitivity (Ultrasensitive Analysis).- 3.6. Superefficient Analysis.- 3.7. Conclusion.- 4. Equipment for Capillary Liquid Chromatography.- 4.1. Specifications.- 4.2. Microbore Liquid Chromatographs.- 4.3. Detectors for Capillary Liquid Chromatography.- 4.3.1. Photometric (Absorbance) Detectors.- 4.3.2. Fluorescence Detectors.- 4.3.3. Refractometers.- 4.3.4. IR Spectrometers.- 4.3.5. Electrochemical Detectors.- 4.3.6. Electrical Conductivity Detectors.- 4.3.7. Potentiometric Detectors.- 4.3.8. Gas Chromatography Detectors.- 4.3.9. Radioactivity Detectors.- 4.3.10. Postcolumn Derivatization.- 4.3.11. Other Sorts of Detectors.- 4.3.12. Liquid Chromatograph/Mass Spectrometer.- 4.3.12a. Detection Limit of a Mass Spectrometer when Used as a Detector.- 4.3.12b. Mass Spectrometer’s Time Constant.- 4.3.12c. Eluent for a Liquid Chromatograph/ Mass Spectrometer.- 4.3.12d. Interface between a Liquid Chromatograph and a Mass Spectrometer.- 4.3.12e. Chromatographic Columns and Separation Systems That Can Be Used with Microbore Liquid Chromatographs Coupled to Mass Spectrometers.- 4.4. Devices for Injecting and Concentrating Samples.- 4.5. Solvent Delivery Systems.- 4.6. Temperature Gradients for Capillary Chromatography..- 5. Preparing and testing capillary columns for liquid Chromatography.- 5.1. Experimental Methods for Determining the Peak Variance Associated with Extracolumn Band Spreading.- 5.2. Packed Microbore Columns. Relationship between Performance and Packing Method.- 5.2.1. Influence of Column Diameter on the Height of a Theoretical Plate. Wall Effect.- 5.2.2. Packing Microbore Columns.- 5.3. Preparing and Testing Microcapillary Columns.- 5.3.1. Packed Capillary Columns with Irregular Packing.- 5.3.2. Open Tubular Columns.- 5.4. Possible Future Increases in the Performance of Capillary Columns.- 5.4.1. Microbore Supercritical-Fluid Chromatography.- 6. Application of Microbore Chromatography to the Analysis of Organic and Inorganic Compounds.- 6.1. Amino Acids, Their Derivatives, Peptides, and Proteins.- 6.1.1. Ultrasensitive Analyses of Amino Acids and Their Derivatives with Fluorometric Detection.- 6.1.2. Microbore Chromatography of PTH Amino-Acid Derivatives.- 6.1.3. Ultrasensitive Analyses of Amino Acids and Peptides with a Postcolumn Ninhydrin Reaction.- 6.1.A. Ultrasensitive Analyses of Amino Acids and Amines (Postcolumn Derivatization with o-Phthalic Dialdehyde).- 6.1.5. Microbore Steric-Exciusion Chromatography of Large Peptides.- 6. 1.6. Reversed-Phase Chromatography of Proteins in Short Microbore Columns.- 6.2 Steric-Exclusion Microbore Chromatography Applied to the Study of Protein Association.- 6.3. Microbore Column Chromatography of Polymers and Oligomers.- 6.3.1. Molecular Weight Distribution of Polymers.- 6.3.2. High-Performance Microbore Liquid Chromatography of Oligomers.- 6.4. Analyses of Antibiotics and Pharmaceuticals.- 6.4.1. Antibiotics.- 6.4. 2. Pharmaceuticals.- 6.4.3. Vitamins.- 6.5. Analyses of Nucleic Acid Components.- 6.6. Analyses of Medicines and Biologically Active Compounds.- 6.6. 1. Direct Microbore Analysis of Biologically Active Compounds and Pharmaceuticals in Biological Fluids.- 6.6.1a. Eicosanoids in Tissue Extracts.- 6.6.1b. Bethanidine in Blood Plasma.- 6.6.1c. Rapid Analyses of Theophylline in Blood Serum.- 6.6.Id. Tyrosine and Tryptophan Metabolites in Urine.- 6.6.2. Ultrasensitive Microbore Analyses of Concentrated Samples.- 6.6.2a. Analyses of Corticosteroids in Blood Serum Using Off-Line Precolumns.- 6.6.2b. Analyses of Catecholamines in Biological Fluids Using Automatic On-Line Concentration.- 6.6.2c. Determination of Nitrophenol in Urine.- 6.6.2d. Blood Serum Analyses Using Sample Concentration and Serial Loop Injectors.- 6.6.3. Analyses Using Precolumn Derivatization for Medicines and Their Metabolites.- 6.6.3a. Glycosides and Their Metabolites in Blood and Urine.- 6.6.3b. Other Investigations.- 6.6.4. Postcolumn Derivatization for Bile Acid Assays.- 6.7. Microbore Liquid Chromatography in Environmental Monitoring.- 6.7.1. Analyzing the Content of Polycyclic and Nitropolycyclic Hydrocarbons in Diesel Fuel.- 6.7.2. Polycyclic Hydrocarbons and Chlorinated Phenols in Water.- 6.7.3. Polycyclic Aromatic Hydrocarbons in Exhaust Fumes.- 6.7.4. Organic Impurities in Water, Given Sample Concentration in Serial Loop Injectors.- 6.7.4a. General Assay for Organic Compounds.- 6.7.4b. Nitrobenzene in River Water.- 6.7.5. Analysis of Phthalic Acid Esters in River Water Using Off-Line Sample Concentration.- 6.7.6. Antioxidants in Gasoline.- 6.7.7. Hydrocarbons in Coal Extracts.- 6.8. Microbore Liquid Chromatography Applied to Inorganic Compounds.- 6.8.1. Halide Ions.- 6.8.2. Alkali Metals.- 6.8.3. Rare-Earth Elements.- 6.8.4. Metal Chloro Complexes.- 6.8.5. Nitrates in Water.- 6.8.6. Ultramicrobore Analyses of Inorganic Ions Using a UV Detector.- 7. Conclusion.- References.