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作 者:许有威[1] 齐艳[1] 韩旭[1] 许丽娜[1] 徐奇玮[1] 彭金咏[1]
出 处:《中国中药杂志》2007年第24期2595-2597,共3页China Journal of Chinese Materia Medica
摘 要:目的:建立龙胆中高纯度龙胆苦苷的快速分离制备方法。方法:药材醇提取液经D101大孔吸附树脂柱的层析物直接进行高速逆流色谱(high-speed counter-current chromatography,HSCCC)分离纯化,以醋酸乙酯-正丁醇-水(2∶1∶3)为溶剂系统,下相为流动相,流速1.5 mL.min-1,检测波长254 nm,分离温度30℃,所得产物经高效液相色谱与质谱分析检测,并与标准品对照。结果:在此条件下,经一步分离从300 mg粗提物中得到136 mg纯度为99.6%的龙胆苦苷。结论:该法简便、快速、所得产物纯度高,适合于龙胆苦苷标准品的制备。Objective: To develop a method for the preparative separation of gentiopicrin from Radix Gentianae by high-speed counter-current chromatography (HSCCC). Method: The crude alcohol extracts were eluted on a macroporous resin column and then purified by high speed counter-current chromatography (HSCCC). A two-phase solvent system composed of ethyl acetate: n-butanol: water (2: 1: 3) was used, and the lower phase was used as the mobile phase at a flow rate of 1.5 mL · min^-1 , while the apparatus rotated at 800 r · min^-1 and the eluate was detected at 254 nm. Result: 136 mg gentiopicrin with purity of 99.6% determined by HPLC were obtained from 300 mg crude extraction only in one-step separation and less than 200 minutes. Conclusion: The established method is simple, high efficiency and suitable for large-scale separation of gentiopicrin.
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