Determination of aminoheterocycle and azabicycle in gliclazide bulk by capillary zone electrophoresis with amperometric detection.

摘要

A simple, reliable and reproducible method, based on capillary zone electrophoresis with amperometric detection (CZE-AD), was developed for simultaneous determination of 3-amino-3-azabicyclo[3,3,0]octane (aminoheterocycle) and 3-azabicyclo[3,3,0]octane (azabicycle) in gliclazide bulk drug. The optimal conditions of CZE-AD were 50 mM borate solution (pH 9.0) as running buffer, 14 kV as separation voltage and 0.95 V (versus SCE) as detection potential. Under the selected optimum conditions, the two analytes could be perfectly separated within 9 min. The linearity range of aminoheterocycle was from 1.0 x 10(-6) to 1.0 x 10(-3) M and that of azabicycle was from 2.0 x 10(-6) to 1.0 x 10(-3) M. Their detection limits were 5.0 x 10(-7) and 1.0 x 10(-6) M, respectively, (S/N=3). This proposed method demonstrated long-term stability and reproducibility with relative standard deviations of less than 2% for both migration time and peak current. It has been successively used for the determination of these two analytes in gliclazide bulk drug, and the assay results were satisfactory.