Wyniki wyszukiwania - BazTech

1

Fingerprint of ethyl acetate extraction combined with qualitative and quantitative analysis on Patrinia scabra Bunge: Distinguish P. scabra Bunge from its confusable species

Liu W., Wei M. L, Wu Ch. Y, Zhu H. Y, Feng F, Xie N

Acta Chromatographica

|

2015

|

Vol. 27, no. 1

177--187

EN

Patrinia scabra Bunge has long been used in clinic as a traditional Chinese medicine for treating leukemia and cancer and regulating host immune response. Despite their wide use in China, no report on system analysis on their chemical constituents is available so far. The current study was designed to profile the fingerprint of ethyl acetate extract of it, and in addition, to characterize the major fingerprint peaks and determine their quantity. Therefore, a detailed gradient high-performance liquid chromatography was described to separate more than 30 compounds with satisfactory resolution in P. scabra Bunge. Based on the chromatograms of 10 batches samples, a typical high-performance liquid chromatographic (HPLC) fingerprint was established with 23 chromatographic peaks being assigned as common fingerprint peaks. Furthermore, a quadrupole time of flight mass spectrometry (Q-TOF/MS) was coupled for the characterization of major compound. As (+)-nortrachelogenin was the most predominant compound in P. scabra Bunge, the quantification on it was also carried out with the method being validated. As a result, (+)-nortrachelogenin was found to be from 1.33 to 2.21 mg g−1 in this plant material. This rapid and effective analytical method could be employed for quality assessment of P. scabra Bunge, as well as pharmaceutical products containing this herbal material.

2

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

EN

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).

3

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

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.