Chemical Derivatization in Analytical Chemistry: Chromatography

ISBN-13: 9781461591962 / Angielski / Miękka / 2012 / 344 str.

R. W. Frei

Opis

The first volume in this series is devoted to derivatization techniques in chromatography, for very obvious reasons. In gas chromatography (GC) chemical derivatization as an aid to expand the usefulness of the technique has been known for more than a decade and has become an established approach. The first chapter deals to a great extent with derivatization for the purpose of making compounds amenable to Gc. Although the discussion concentrates on pesticides, some generally valid conclusions can be drawn from this chapter. Chemistry will not be limited to the separation-it can also have a pronounced impact on the sample cleanup, another topic cov- ered in Chapter 1. Since the introduction of coupled GC-mass spectroscopy (GC-MS), a very powerful tool, derivatization techniques have taken still another di- rection-taking into consideration chromatographic as well as mass spec- trometric improvement of the compounds of interest. Cyclic boronates are discussed as derivatization reagents for this purpose in the second chapter.

Spis treści

1. Chemical Derivatization in Pesticide Analysis.- 1. Introduction.- 2. Organochlorine Insecticides.- 2.1. The DDT Group.- 2.2. Cyclodiene Insecticides.- 2.3. Miscellaneous.- 2.4. Cleanup Techniques Using Chemical Reactions.- 3. Organophosphorus Insecticides.- 3.1. Derivatization of the P Moiety.- 3.2. Derivatization of the Alkyl or Aryl Moiety.- 3.3. On-Column Transesterification.- 3.4. Derivatization of the Intact Insecticide.- 4. Carbamates (Insecticides and Herbicides).- 4.1. Hydrolysis and Derivatization of the N Moiety.- 4.2. Hydrolysis and Derivatization of the Alkyl or Aryl Moiety.- 4.3. On-Column Methylation.- 4.4. Derivatization of the Intact Carbamate.- 5. Herbicides.- 5.1. Triazines.- 5.2. Ureas.- 5.3. Chlorophenoxy Acids.- 5.4. Miscellaneous.- 6. Phenols.- 7. Fungicides.- References.- 2. Cyclic Boronates as Derivatives for the Gas Chromatography—Mass Spectrometry of Bifunctional Organic Compounds.- 1. Introduction.- 2. Some Historical Background.- 3. The Scope of Application of Cyclic Boronates in Gas Chromatography.- 4. Gas Chromatographic Properties of Cyclic Boronates.- 5. Mass Spectrometric Properties of Cyclic Boronates.- 6. Preparation of Cyclic Boronates for Use in Gas Chromatography-Mass Spectrometry.- 7. Examples of the Preparation and Gas Chromatography of Cyclic Boronates...- 8. Summary.- References.- 3. General Aspects of Precolumn Derivatization with Emphasis on Pharmaceutical Analysis.- 1. Introduction.- 1.1. Purposes for Derivatization.- 1.2. HPLC Detectors and Compatible Derivatives.- 1.3. Chemical Reactions Used in Derivatization.- 2. Functional Group Analysis.- 2.1. Amines.- 2.2. Alcohols and Phenols.- 2.3. Carboxylic Acids.- 2.4. Aldehydes and Ketones.- 2.5. Miscellaneous Nitrogen-Containing Compounds.- 2.6. Thiols.- 3. Detector Amplification by Paired Ion Chromatography.- 3.1. Theoretical Considerations.- 3.2. Applications.- 4. Conclusions.- References.- 4. Reaction Detectors in Liquid Chromatography.- 1. Introduction.- 2. Theoretical Aspects.- 2.1 Tubular Reactors.- 2.1. Bed Reactors.- 2.2. Segmented Stream Reactors.- 2.3. Mixing Units.- 3. Technical Aspects and Applications.- 3.1. Tubular Reactors (Nonsegmented Streams).- 3.2. Bed Reactors.- 3.3. Segmented Stream Reactors.- 4. Special Applications and Trends.- 4.1. Coupling with Other Detection Modes.- 4.2. Coupling with Other Techniques.- 5. Conclusions.- References.