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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.

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Several polymer-bound o-nitrobenzophenone reagents containing different detector-sensitive tags have been combined in the same reactor for the on-line derivatization of amine samples. The formation of multiple derivatives allows numerous opportunities for quantitation from the same injection, and also allows improved identification from the retention times of the multiple derivatives. Changing the reaction conditions changes the ratio of the products formed, so that changes in the ratio of peak heights and areas can also be used for analyte identification. In this work, propylamine was derivatized in acetonitrile on-line, precolumn. Changing the reaction conditions, of reaction time, temperature, solvent, presence of catalyst and the components of the reactor, changed the ratio of the derivatives formed. These changes in product formation with changing reaction conditions were applied to the identification and quantitation of amphetamine and methamphetamine in urine. The drugs were identified by the retention times of their derivatives, the ratio of the peak areas of the derivatives and the change in the ratios after changing reaction conditions. Each derivative was also used for quantitation of levels of spiked concentrations of amphetamine and methamphetamine, with relative errors less than 8%.