Polymeric reagents for derivatizations in micellar electrokinetic chromatography

Abstract

A polymer immobilized o-nitrobenzophenone reagent was prepared for analysis of amine drugs in micellar electrokinetic chromatography (MEKC). A model compound, propylamine, was used to characterize the reagent's performance in MEKC. Derivatizations were performed on the CE instrument with reagent in the sample vial. The yielded derivative was directly sampled from the reaction mixture, and directly injected onto the MEKC system. The derivatization reagent was also applied to the derivatization of n-alkyl amine mixtures and amino acids. The method was validated for adamantanamine in urine and in plasma by single-blind spike analysis. Precisions and accuracies for all samples were less than 6.0% for urine samples and 10% for plasma samples. The procedure was a direct injection technique requiring minimal sample preparation for the analysis of drugs in biofluids.

Size-selective Derivatizations with Polymer Immobilized Reagents

“…Pore sizes of supports have been measured indirectly, using reverse size exclusion chromatography (SEC) with both silica (Warren and Bidlingmeyer, 1984) and polymeric (Jerabek et al, 1992) supports. SEC is performed with well characterized supports of known pore sizes in order to determine the molecular weight of an eluting analyte.…”

“…These reagents have been used in HPLC for the on-line determination of chiral (Chou et al, 1989) and achiral amine drugs (Gao et al, 1989), amino acids (Bourque and Krull, 1991), and peptides (Zhou et al, 1993a). Other applications include combining several reagents in a reactor to form a multiple derivatives precolumn, so that each of these derivatives may be used to quantitate and confirm the presence of an analyte (Szulc and Krull, 1992). Also, since the reagents are compatible with biological fluids, an analyte in urine or plasma may be derivatized without extraction, with no interference from derivatized protein components.…”

“…Also, since the reagents are compatible with biological fluids, an analyte in urine or plasma may be derivatized without extraction, with no interference from derivatized protein components. Thus, these reagents are practical for direct injection of analytes in biofluids in either HPLC (Zhou et al, 1993b, c) or micellar electrokinetic chromatography (Szulc and Krull, 1994).…”

Development and applications of a post-column reaction system for fluorescence detection in capillary electrophoresis

“…To prevent the reagent from flowing into the separation capillary, the pressure is applied on the reagent reservoir and separation capillary inlet simultaneously. A microfluorescence detector with a Xe-Hg lamp for excitation was used for fluorescence detection.In a pressure driven system, the zone broadening by the laminar flow is proportional to the square of the inner diameter of the reaction capillary and to the reaction time (Zhu and Kok, 1995). Therefore the derivatization reactions should have fast kinetics.…”

“…Several post-column reaction systems have been developed for CE including co-axial reactors, gap reactors, sheath flow reactors etc. (Szulc and Krull, 1994). For routine analysis, a simple, repeatable and easy to use post-column reaction system is required.…”