曲克芦丁原料药中三羟乙基芦丁及相关物质的半制备液相色谱法分离纯化
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摘要
通过半制备液相色谱法对曲克芦丁原料药中三羟乙基芦丁及相关物质进行分离纯化。采用C18色谱柱,分别以乙腈-水(17∶83,V/V)和甲醇-水(60∶40,V/V)为流动相,流速为1.0mL·min-1,检测波长254nm。经高效液相色谱法分离分析,制备的3个化合物的纯度均在98%以上,经核磁共振、质谱等分析检测,推断它们分别为三羟乙基芦丁、四羟乙基芦丁和四羟乙基槲皮素。该制备方法简便高效,重现性好,对进一步提高和监控曲克芦丁产品的质量具有重要意义。
Drug substance of troxerutin was isolated and purified by semi-preparative liquid chromatography to prepare trihydroxyethylrutin and other related substances.The preparation was performed on C18 column with the mobile phase consisting of acetonitrile-water(17∶83,V/V)or methanol-water(60∶40,V/V),the flow-rate was 1.0 mL·min-1 and detection wavelength was set at 254 nm.The purity of the three compounds which were prepared by semi-preparative liquid chromatography were all above 98%.According to the NMR and MS analysis,they were preliminarily estimated to be trihydroxyethylrutin, tetrahydroxyethylrutin and tetrahydroxyethylquercetin,respectively.The method was simple,efficient,reproducible and suitable for preparing trihydroxyethylrutin and related substances from drug substance of troxerutin.
Drug substance of troxerutin was isolated and purified by semi-preparative liquid chromatography to prepare trihydroxyethylrutin and other related substances.The preparation was performed on C18 column with the mobile phase consisting of acetonitrile-water(17∶83,V/V)or methanol-water(60∶40,V/V),the flow-rate was 1.0 mL·min-1 and detection wavelength was set at 254 nm.The purity of the three compounds which were prepared by semi-preparative liquid chromatography were all above 98%.According to the NMR and MS analysis,they were preliminarily estimated to be trihydroxyethylrutin, tetrahydroxyethylrutin and tetrahydroxyethylquercetin,respectively.The method was simple,efficient,reproducible and suitable for preparing trihydroxyethylrutin and related substances from drug substance of troxerutin.
引文
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