高速逆流色谱法分离制备枳壳中水合橘皮内酯等3个标准物质的研究  

Studies on separation and preparation of 3 standard materials such as meranzin hydrate from the Fructus Aurantii by high-speed counter-current chromatography

作　　者：宋玉鹏[1] 董晶[1] 陈海芳[1] 胡源祥 谭舒舒 杨武亮[1] 

机构地区：[1]江西中医药大学现代中药制剂教育部重点实验室,南昌330004

出　　处：《药物分析杂志》2017年第1期137-141,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然科学基金资助项目(编号:81460575;81260612);江西中医药大学校级研究生创新项目(JZYC15S43)

摘　　要：目的:采用高速逆流色谱法从枳壳中分离制备高纯度的水合橘皮内酯、川陈皮素和橘皮素。方法:枳壳用乙醇回流提取,经三氯甲烷萃取得到萃取物,再应用制备型高速逆流色谱仪,通过优化各分离条件,以石油醚-乙酸乙酯-甲醇-水(10:9:7:8)四元两相溶剂系统上相为固定相,下相为流动相,高速逆流色谱仪转速880 r·min^(-1),流动相流速2 mL·min^(-1),制备分离枳壳三氯甲烷萃取部分粗提物,所得产物的纯度经HPLC检测,结构经EI-MS、~1H-NMR和^(13)C-NMR鉴定。结果:100 mg粗提物经270min 1次分离制备得到了3个化合物,鉴定为水合橘皮内酯、川陈皮素和橘皮素,称量,水合橘皮内酯8.8 mg、川陈皮素7.3 mg和橘皮素4.7mg,采用峰面积归一化法计算其质量分数分别为96.70%、97.89%和98.52%。结论:由该法从枳壳中分离制备水合橘皮内酯、川陈皮素和橘皮素简便、经济,所得化合物纯度高,可作为枳壳药材质量控制的参考物质。Objective： To establish a method for preparative separation of meranzin hydrate, nobiletin and tangeretin with high purity from Fructus Aurantii by high-speed counter-current chromatography （ HSCCC ）. Methods： After various parameters of preparative HSCCC were optimized preliminarily, the chloroform crude extract of the Fructus Aurantii was separated with a two-phase solvent system composed of light petroleumethyl acetate-methanol-water（ 10：9：7 ： 8 ）. The flow rate was 2 mL·min-1, and the rotation rate was 880 r·min-1. The upper phase was chosen as the stationary phase, while the lower phase was chosen as the mobile phase. The purity of compounds obtained were analyzed by HPLC, and the structures of the compounds were identified by El-MS, 1H-NMR and 13C-NMR. Results： Three compounds, including 8.8 mg of meranzin hydrate, 7.3 mg of nobiletin and 4.7 mg of tangeretin were obtained from 100 mg crude sample in one-step separation in 270min. The mass fraction were 96.70%, 97.89% and 98.52% respectively by using the peak area normalization method. Conclusion： The established HSCCC method is simple and feasible, which can be used for rapid preparative isolation of the meranzin hydrate, nobiletin and tangeretin from Fructus Aurantii. The compounds obtained in tile experiment can be used as reference materials for quality control of Fructus Aurantii.

关 键 词：枳壳 水合橘皮内酯 川陈皮素 橘皮素 对照品制备 高速逆流色谱(HSCCC) 标准物质 

分 类 号：R917[医药卫生—药物分析学]