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目的:建立高速逆流色谱法高效、快速分离制备化橘红中3个主要成分柚皮苷、橙皮内酯水合物、异橙皮内酯的新方法。方法:化橘红用9 5%乙醇超声提取,经石油醚(6 0~9 0℃)、二氯甲烷、正丁醇分级萃取初步分离,再进行高速逆流色谱分离。石油醚层所用的溶剂体系为正己烷-乙酸乙酯-甲醇-水(1∶1∶1∶1),二氯甲烷层所用的溶剂体系为正己烷-乙酸乙酯-甲醇-水(1∶2∶1∶2.5),正丁醇层所用两相溶剂体系为乙酸乙酯-正丁醇-水(4∶1∶5),高速逆流色谱仪转速8 5 7 r.min-1,所得产物的纯度经HPLC检测,结构经NMR和M S鉴定。结果:从化橘红粗提物中分离得到纯度高于9 8.0%的柚皮苷、橙皮内酯水合物,纯度高于9 5.0%的异橙皮内酯,得率均高于2 5%。结论:由该法从化橘红中制备柚皮苷、橙皮内酯水合物、异橙皮内酯简便、快速,所得产物纯度高,适合于其对照品的大规模制备。
OBJECTIVE: To establish a new method for the rapid and efficient separation and separation of naringin, cumarone hydrate and isocynanolactone from three major constituents of Radix Angelicae Sinensis by high-speed countercurrent chromatography. Methods: The orange juice was extracted by ultrasonic with 95% ethanol and separated by petroleum ether (60 ~ 90 ℃), methylene chloride and n-butanol fractional extraction, and then separated by high speed countercurrent chromatography. The solvent system for the petroleum ether layer was n-hexane-ethyl acetate-methanol-water (1: 1: 1: 1) and the solvent system for the dichloromethane layer was n-hexane-ethyl acetate-methanol- 2: 1: 2.5). The two-phase solvent system of n-butanol was ethyl acetate-n-butanol-water The purity was determined by HPLC. The structure was identified by NMR and MS. Results: Naringin and cumarone hydrate with the purity of more than 9 8.0% were isolated from the orange extract, and the isoquercoides with the purity higher than 95.0% were obtained. The yield was higher than 25%. Conclusion: The naringin, apigenol hydrate and isocynanolactone prepared from the tangerine extract by this method are simple and rapid. The obtained product has high purity and is suitable for the large-scale preparation of its reference substance.