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

• Autorzy: Liu W.-Y , Yang X.-J , Li P. , Feng F , Mao L.
• Języki publikacji: EN

Abstrakty

EN

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.

Słowa kluczowe

EN

column liquid chromatography; quantitative analysis; 10-O-(N, N-dimethylaminoethyl)-ginkgolide B (XQ-1); related impurities

• Wydawca: University of Silesia in Katowice ; Akademiai Kiado
• Czasopismo: Acta Chromatographica
• Rocznik: 2011
• Tom: Vol. 23, no. 3
• Strony: 459--468
• Opis fizyczny: Bibliogr. 5 poz., rys., tab.

Twórcy

autor

Liu W.-Y

• China Pharmaceutical University Department of Pharmaceutical Analysis Nanjing 210009 China
• China Pharmaceutical University, Ministry of Education Key Laboratory of Drug Quality Control and Pharmacovigilance Nanjing 210009 China

autor

Yang X.-J

• China Pharmaceutical University Department of Pharmaceutical Analysis Nanjing 210009 China

autor

Li P.

• China Pharmaceutical University Department of Pharmaceutical Analysis Nanjing 210009 China

autor

Feng F

• China Pharmaceutical University Department of Phytochemistry Nanjing 210009 China

autor

Mao L.

• Jiangsu Carefree Medicinal Company Limited Nanjing 210016 China

Bibliografia

• [1] L.H. Hu, Z.L. Chen, Y.Y. Xie, Y.Y. Jiang, and H.W. Zhen, Bioorg. Med. Chem., 8, 1515 (2000)
• [2] K.M. Maclennan, C.L. Darlington, and P.F. Smith, Prog. Neurobiol., 67, 235 (2002)
• [3] B. Ahlemeyer and J. Krieglstein, Cell. Mol. Life Sci., 60, 1779 (2003)
• [4] Y. Deng, W.R. Fang, Y.M. Li, J. Cen, F. Fang, P. Lv, S.B. Gong, and L.S. Mao, Eur. J. Pharmacol., 616, 43 (2009)
• [5] W.Y. Liu, P. Li, F. Feng, and L.S. Mao, J. Pharm. Biomed. Anal., 52, 603 (2010)