A summary Is provided of most of Che reported derlvatizations that have been used for improved analyte detection in liquid chromatography with electrochemical detection (LCEC). These approaches include pre-column derivatizations and postcolumns chemical, photochemical or enzymatic reactions for oxidative EC detection. This review covers the literature up to early 1985, and includes information gathered from books, technical articles, previous reviews and scientific journal publications. Specific reagents, methods and instrumentation are described for those classes of compounds studied by derlvatization-LCEC, and suggestions for future experiments are included, where applicable. It is concluded that the future will likely Include the development of a great number of derivatizations which may be used in conjunction with LCEC for trace analysis.

Derivatization and Post-Column Reactions for Improved Detection in Liquid Chromatography/Electrochemistry

This article describes both pre- and postcolumn derivatization chemistry used in conjunction with either chromatography or capillary electrophoresis (CE) to facilitate the determination of drugs. Generally, only prederivatization is used in gas chromatography (GC), principally to enhance the volatility, temperature stability, and/or detectability. The GC section considers derivatization of drugs by reagent class: alkylation, acylation, and silylation. The GC sample-handling section describes an approach that combines the extraction and derivatization steps together. Both pre- and postcolumn derivatization are common approaches for high-performance liquid chromatography (HPLC) and many of these methods have been adapted for CE. Derivatization for HPLC is often directed toward aliphatic amines, carboxylic acids, or alcohols that are difficult to detect at low levels by absorbance, luminescence, or electrochemical means. In addition, small hydrophilic molecules upon prederivatization are often converted into larger more hydrophobic compounds, making reversed-phase HPLC easier or even feasible. The HPLC section considers derivatization of drugs based on the following types: alkaloids, amines, antibiotics, barbiturates, carbonyl compounds and carboxylic acids, catecholamines, hydroxy compounds, steroids, and sulfur compounds. For the GC and HPLC sections, tables are included, giving the structures of the more important derivatizing agents, the analytes, and the corresponding reaction products. A brief rationale for derivatization chemistry with CE concludes this article. For CE, derivatization is often done to improve detectability as the path length for absorbance detection is very short and fluorescence can be effective using laser-based systems.

Chemical Reagents and Derivatization Procedures in Drug Analysis

As in all other forms of chromatography, high performance liquid chromatography (HPLC) has come to rely quite heavily on derivatization of individual analytes for improved qualitative and quantitative identifications (1–13). Virtually all of this work has involved the use of homogeneous type derivatizations, wherein the sample solution to be injected, in the pre-column approach, or the HPLC effluent, in the post-column approach, are fully mixed with the derivatization reagents in solution. Clearly, homogeneous type derivatizations can be done off-line or on-line, in either the pre-or post-column modes, but in general, pre-column methods have been done offline, and post-column approaches have been done both on-line and off-line. Online type derivatizations, in either the pre-or post-column modes, appear to offer some very significant advantages. Major among these is the ability to perform derivatization-separation-detection or separation-derivatization-detection following injection of the sample m...

Solid Phase Reactions for Derivatization in Hplc (HPLC-SPR)

This paper describes an H.P.L.C. method for the assay of gentamicin sulphate, utilising pre-column derivatisation with an ophthalaldehyde/thioglycollic acid reagent, ion-paired chromatography of th...

The Analysis of Gentamicin Sulphate in Pharmaceutical Specialities by High Performance Liquid Chromatography

Dehydrogenation of 2-trimethylsilyl-1-propanol (1) was carried out with horse liver alcohol dehydrogenase (HLADH, EC 1.1.1.1). It was found that the hydrogenation of 1 proceeded enantioselectively with only HLADH and a catalytic amount of NAD+ due to in-situ NAD+ regeneration based on a specific property of β-carbonylsilanes. That is, (+)-1 was enantioselectively dehydrogenated by HLADH to 2-trimethylsilyl-1-propanal, which was spontaneously degraded by addition of water into trimethylsilanol and n-propanal. Then, NAD+ was regenerated through HLADH-catalyzed reduction of n-propanal to n-propanol. On the other hand, dehydrogenation of the carbon analogue of 1 was negligible with a catalytic amount of NAD+, indicating that the in-situ NAD+ regeneration was not available without the specific property of organosilicon compounds. Other primary β-hydroxysilanes having different substituents on the chiral center or on the silicon atom were also found to serve as substrates in enantioselective dehydrogenation by HLADH with this novel NAD+ regeneration system. Chiral recognition of HLADH toward primary alcohols is also discussed.

Enantioselective dehydrogenation of β-hydroxysilanes by horse liver alcohol dehydrogenase with a novel in-situ NAD+ regeneration system

Chemical derivatization for the liquid chromatography of compounds of pharmaceutical interest.

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Chemical derivatization for the liquid chromatography of compounds of pharmaceutical interest.