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Won O. Song and Gary R. Beecher are the authors of Modern Analytical Methodologies in Fat- and Water-Soluble Vitamins, published by Wiley.

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Modern Analytical Methodologies in Fat- and Water-Soluble Vitamins

John Wiley & Sons

Copyright © 2000 Won O. Song
All right reserved.
ISBN: 978-0-471-17942-9

Contents

CONTRIBUTORS...........................................................................................................................................xvPREFACE................................................................................................................................................xviiCUMULATIVE LISTING OF VOLUMES IN SERIES................................................................................................................xixPART 1 FAT-SOLUBLE VITAMINSCHAPTER 1 VITAMIN A Thomas Arnhold, Heinz Nau, and Ralph Ruehl........................................................................................31.1. Introduction......................................................................................................................................31.2. Sample Collection, Handling, and Storage..........................................................................................................71.3. Sample Preparation................................................................................................................................81.4. Reference Standards...............................................................................................................................151.5. High-Performance Liquid Chromatography............................................................................................................161.6. Other Liquid Chromatographic Methods..............................................................................................................341.7. Gas Chromatography................................................................................................................................351.8. Capillary Electrophoresis.........................................................................................................................361.9. Bioassays.........................................................................................................................................39References.............................................................................................................................................39CHAPTER 2 VITAMIN D Michael F. Holick.................................................................................................................512.1. Origins of Vitamin [D.sub.2] and Vitamin [D.sub.3]................................................................................................512.2. Metabolism and Biologic Functions of Vitamin D....................................................................................................542.3. Measurement of Vitamin D Bioactivity..............................................................................................................552.4. Modern Methods for Determining the Vitamin D Content in Blood.....................................................................................552.5. Strategies for Determining Circulating Concentrations of 25-Hydroxyvitamin D......................................................................562.6. Strategies for Determining Circulating Concentrations of 1,25-Dihydroxyvitamin D..................................................................662.7. Measurement of 24,25-Dihydroxyvitamin D and 25,26-Dihydroxyvitamin D..............................................................................732.8. Clinical Utility for Assays for Vitamin D and Its Metabolites.....................................................................................742.9. Conclusion........................................................................................................................................76References.............................................................................................................................................77CHAPTER 3 DETERMINATION OF TOCOPHEROLS AND TOCOTRIENOLS IN FOODS AND TISSUES Vieno I. Piironen.......................................................813.1. Introduction......................................................................................................................................813.2. Vitamin E Compounds in Foods and Tissues..........................................................................................................823.3. High-Performance Liquid Chromatography............................................................................................................853.4. Gas Chromatography................................................................................................................................1123.5. Supercritical Fluid Extraction and Chromatography.................................................................................................1123.6. Determination of Stereoisomers....................................................................................................................1133.7. Future Development................................................................................................................................114References.............................................................................................................................................115CHAPTER 4 VITAMIN K Sarah L. Booth, Kenneth W. Davidson, James A. Sadowski, and Gregory G. Dolnikowski................................................1294.1. Introduction......................................................................................................................................1294.2. Determination of Phylloquinone by HPLC............................................................................................................1334.3. Determination of Phylloquinone Metabolites and Hydrogenation Products.............................................................................1464.4. Determination of Menaquinones by HPLC.............................................................................................................1534.5. Other Indicators of Vitamin K Nutritional Status..................................................................................................1554.6. Summary...........................................................................................................................................158References.............................................................................................................................................160CHAPTER 5 SIMULTANEOUS DETERMINATION OF FAT-SOLUBLE VITAMINS IN FOOD, FEED, AND SERUM Ronald R. Eitenmiller and W. O. Landen, Jr......................1715.1. Introduction......................................................................................................................................1715.2. Simultaneous Analysis of Fat-Soluble Vitamins in Food and Feed....................................................................................1725.3. An Integrated Approach to Fat-Soluble Vitamin Analysis of Foods...................................................................................1935.4. Simultaneous Analysis of Fat-Soluble Vitamins in Serum or Plasma..................................................................................1955.5. Concluding Comments...............................................................................................................................215References.............................................................................................................................................215PART 2 WATER-SOLUBLE VITAMINSCHAPTER 6 THIAMIN Ronald R. Eitenmiller and W. O. Landen, Jr..........................................................................................2256.1. Introduction......................................................................................................................................2256.2. Properties........................................................................................................................................2266.3. Methodology.......................................................................................................................................2296.4. Conclusion........................................................................................................................................246References.............................................................................................................................................246CHAPTER 7 RIBOFLAVIN Ronald R. Eitenmiller and W. O. Landen, Jr.......................................................................................2537.1. Introduction......................................................................................................................................2537.2. Properties........................................................................................................................................2547.3. Methodology.......................................................................................................................................2587.4. Concluding Comments...............................................................................................................................278References.............................................................................................................................................283CHAPTER 8 VITAMIN [B.sub.6] Stephen P. Coburn.........................................................................................................2918.1. Introduction......................................................................................................................................2918.2. Processing of Standards and Samples...............................................................................................................2918.3. Fluorometric Methods..............................................................................................................................2948.4. Enzymatic Methods.................................................................................................................................2958.5. Gas Chromatography/Mass Spectrometry..............................................................................................................2958.6. High-Performance Liquid Chromatography............................................................................................................2968.7. Electrophoresis...................................................................................................................................2998.8. Microbiological Assay.............................................................................................................................2998.9. Immunoassay.......................................................................................................................................3018.10. 4-Pyridoxic Acid.................................................................................................................................3018.11. Other Metabolites................................................................................................................................3018.12. Assessment of Vitamin B6 Status..................................................................................................................3028.13. Conclusions......................................................................................................................................304References.............................................................................................................................................305CHAPTER 9 VITAMIN [B.sub.12] Edward V. Quadros........................................................................................................3139.1. Introduction......................................................................................................................................3139.2. Cobalamin Binding Proteins........................................................................................................................3159.3. Materials.........................................................................................................................................3169.4. Preparation of Binding Proteins...................................................................................................................3179.5. Standardization of Binding Proteins...............................................................................................................3199.6. Extraction of Cbl from Serum or Plasma............................................................................................................3209.7. Extraction of Cbl from Cells or Tissues...........................................................................................................3209.8. Assay Protocol....................................................................................................................................3219.9. General Comments on Assay Protocol................................................................................................................3229.10. Interpretation of Results........................................................................................................................323References.............................................................................................................................................325CHAPTER 10 NIACIN Shunitz Tanaka.....................................................................................................................32910.1. Introduction.....................................................................................................................................32910.2. General Methods..................................................................................................................................33110.3. High-Performance Liquid Chromatography...........................................................................................................33210.4. Capillary Electrophoresis........................................................................................................................33810.5. Improvement of Chemical and Biological Methods...................................................................................................34110.6. Electrochemical Detection........................................................................................................................343References.............................................................................................................................................346CHAPTER 11 PANTOTHENATE Won O. Song, Carl T. Wittwer, and Bonita W. Wyse..............................................................................35111.1. Biological Importance............................................................................................................................35111.2. Derivatives and Salts of Pantothenic Acid........................................................................................................35911.3. Analytical Methods for Pantothenic Acid..........................................................................................................36511.4. Analytical Methods for Measuring CoA and Intermediates...........................................................................................378References.............................................................................................................................................383CHAPTER 12 BIOTIN Janos Zempleni and Donald M. Mock...................................................................................................38912.1. Introduction.....................................................................................................................................38912.2. Microbiological Assays...........................................................................................................................39212.3. Avidin-Binding Assays............................................................................................................................39312.4. Microbial Versus Avidin-Binding Assays...........................................................................................................39512.5. Chromatographic Procedures.......................................................................................................................39612.6. Radioisotopes of Biotin..........................................................................................................................39712.7. Analysis of Biotin-Dependent Carboxylases........................................................................................................39712.8. Biotin Metabolites in Biological Fluids..........................................................................................................39912.9. Biotin Metabolites in Food.......................................................................................................................400References.............................................................................................................................................402CHAPTER 13 VITAMIN C Steven C. Rumsey and Mark Levine.................................................................................................41113.1. Introduction.....................................................................................................................................41113.2. Stability, Sensitivity, and Substance Interference...............................................................................................41513.3. Colorimetric / Spectrometric Assays..............................................................................................................41713.4. Fluorometric Assays..............................................................................................................................41913.5. GasLiquid Chromatography........................................................................................................................42013.6. Enzymatic Assays.................................................................................................................................42113.7. Capillary Zone Electrophoresis...................................................................................................................42213.8. High-Performance Liquid Chromatography...........................................................................................................42213.9. Assays of Semidehydroascorbic Acid...............................................................................................................43013.10. Flow Injection Assay............................................................................................................................43013.11. In Vivo Assays..................................................................................................................................43113.12. Assay Comparisons...............................................................................................................................43213.13. Summary and Conclusions.........................................................................................................................433References.............................................................................................................................................434INDEX..................................................................................................................................................447

Preface

The role of vitamins in human health is constantly being redefined and expanded. As a result, accurate and precise values for the various forms of each vitamin in small biological samples as well as in foods and beverages are in great demand. This volume constitutes an update of the state of the art of vitamin analysis and highlights new, sensitive analytical procedures for biological samples. Reversed-phase, high-performance liquid chromatography (RP-HPLC), coupled with appropriate detection procedures, constitutes the "workhorse" measurement system for vitamins. This status has been promoted by recent advances in reversed-phase column technology and by advances in HPLC detectors. Where appropriate, the applications of other separation systems, e.g., gas chromatography and capillary zone electrophoresis, are also described. Sample extraction and preparation are time-consuming activities during the analysis of foods and biological samples for vitamins. The applications of new instrumentation, which greatly reduces sample preparation time, are discussed by several authors.

This volume is designed primarily for those who have a familiarity with the different sample preparation and chromatographic techniques. However, each author has provided useful information for a beginner in this field.

This work could not have been presented without the hard work and cooperation of the various authors. We are grateful for their efforts and patience.

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