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A study of impurities and degradation products in Oroxylin A by a validated liquid chromatographic method with analysis of their formation pathways

Liu W.-Y., Xie Sh.-L., Xu X. Zh., Wu Ch. Y., Feng F.

Acta Chromatographica

2013

Vol. 25, no. 3

451--464

Oroxylin A (5,7-dihydroxy-6-methoxyflavone), which has showed multiple pharmacological effects, was semi-synthesized chemically as a pharmaceutical agent. Its impurities, degradation products and their formation pathways remain unknown. In the present study, two impurities (5,6,7-trihydroxyflavone, 5-hydroxy-6,7-dimethoxytlavone) and a degradation product (5,7-dihydroxy-8-methoxyflavone) in Oroxylin A bulk drug substance were identified, and their formation pathways were proposed. A reversed phase liquid chromatographic method for the simultaneous determination of Oroxylin A and the three compounds was developed on a C18 column using methanol-acetonitrile-0.1% acetic acid (54:23:23, v/v/v) as the mobile phase. The detection was performed at 271 nm. The method was validated to be robust, precise, specific and linear between 4 and 40 μg mL-1; the limits of detection and quantification of Oroxylin A were 0.01 and 0.04 μg mL-1, respectively. The developed method was found to be suitable to check the quality of bulk samples of Oroxylin A at the time of batch release and also during its stability studies (long term and accelerated stability).

Simultaneous RP-LC analysis of 10-O-(N,N-dimethylaminoethyl)-ginkgolide B and three related impurities

Liu W.-Y, Yang X.-J, Li P., Feng F, Mao L.

Acta Chromatographica

2011

Vol. 23, no. 3

459--468

10-O-(N,N-dimethylaminoethyl)-ginkgolide B (XQ-1) is an intermediate for synthesizing 10-O-(N,N-dimethylaminoethyl)-ginkgolide B methanesulfonate (XQ-1H), which is a novel ginkgolide B derivative and is being developed as a platelet-activating factor antagonist. A specific and rapid liquid chromatographic method was developed for the quantitative analysis of XQ-1 and its three related impurities, which were 10-O-(N,N-dimethylaminoethyl)-11,12-seco-ginkgolide B (imp-1), 10-O-(N,N-dimethylaminoethyl)-11,12-seco-3,14-dehydroginkgolide B (imp-2) and 10-O-(N,N-dimethylaminoethyl)-3,14-dehydroginkgolide B (imp-3) simultaneously in XQ-1 samples. Chromatographic separation was achieved on a CN band stationary phase, with the mobile phase consisting of methanol and 20 mM dipotassium hydrogen phosphate (pH 7.5) (50:50, υ/υ) in isocratic elution. The flow rate was 1.0 mL min-1 and detector was set at 220 nm. The method was optimized by the analysis of the samples generated during the forced degradation studies. The XQ-1, imp-1, imp-2, and imp-3 were completely separated within 15 min. The resolutions (Rs) amongst four target compounds were >2. The developed method was validated with respect to specificity, linearity, accuracy, precision, and robustness. The results indicated that the simultaneous LC determination method was readily utilized as a quality control method for XQ-1 sample.