Water-promoted formation of phenylboronates of 1,3-diols during gas-liquid chromatographic analysis: application to the assay of meprobamate

ANALYSTANALYST Pub Date: DOI: 10.1039/AN9891400703

Abstract

A simple method for the assay of the hypnotic drug meprobamate (2-methyl-2-propylpropane-1,3-diol dicarbamate) in plasma has been developed. Hydrolysis to the 1,3-diol was followed by extraction into an organic solvent and, after mixing with phenylboronic acid in methanol-water (2 + 1), a portion (1–2 μl) of the extract was analysed directly by gas-liquid chromatography with flame ionisation detection using a column packed with 3%m/m OV-101 at 160 °C. Mebutamate (2-methyl-2-sec-butylpropane-1,3-diol dicarbamate) was used as a reactive internal standard. The limit of accurate measurement was 5 mg l–1[intra-assay coefficient of variation 5.2%(n= 10)] and the assay calibration was linear up to 200 mg l–1. The inter-assay coefficient of variation was 3.7% at 60 mg l–1(n= 10). The finding that water acts to promote phenylboronate formation under the conditions described may prove useful when analysing other 1,2- and 1,3-diols and, possibly, other polar bifunctional compounds by gas-liquid chromatography.

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