Add time:09/26/2019 Source:sciencedirect.com
A capillary gas chromatographic method has been developed to quantitate the Methylboronic acid (cas 13061-96-6) in a lyophilized formulation. The formulation is first dissolved in 1 M hydrochloric acid. Next a tetrahydrofuran solution of the internal standard, 1-butaneboronic acid, and a methylene chloride solution of the derivatizing reagent, pinacol (2,3-dimethyl-2,3-butanediol), are added. The two-phase mixture is shaken for 3 h at 60°C during which time the methylboronic acid is extracted into the methylene chloride phase and reacted with pinacol to form the cyclic pinacol-boronate ester. The product formed in methylene chloride is injected in the split mode onto a capillary gas chromatographic system equipped with a flame ionization detector. Quantitation is achieved by an external standard method.
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