白花败酱草黄酮类成分的高速逆流色谱快速制备

 目的应用高速逆流色谱分离纯化白花败酱草化学成分。方法利用正己烷-乙酸乙酯-甲醇-水(1∶0.6∶0.6∶1)为两相溶剂系统,主机转速800 r·min^-1,上相为固定相,下相为流动相,流速2.0 mL·min^-1,检测波长254 nm,所得产物经高效液相色谱法检测,结构经MS、¹H-NMR和13C-NMR鉴定。结果6 h内经一步洗脱从400 mg白花败酱草乙酸乙酯萃取物中分离得到纯度高于98%的木犀草素26 mg,5-羟基-7,4′-二甲氧基黄酮15 mg和5-羟基-7,3′,4′-三甲氧基黄酮21 mg。结论3个化合物均为首次从败酱属植物中分离得到,该分离制备法简便、快速、产物纯度高。

Isolation and Separation of Flavones from Patrinia villosa by High-Speed Counter-Current Chromatography

OBJECTIVE To develop a preparative high-speed counter-current chromatography(HSCCC) for isolating the chemical constituents from Patrinia villosa Juss.METHODS A two-phase solvent system composed of n-hexane: ethyl acetate: methanol: water(1∶(0.6∶0.6)∶1) was used.at a flow rate of 2.0 mL·min^-1,while the apparatus rotated at 800 r·min^-1 and the effluent was detected at 254 nm.The obtained fractions were analyzed by HPLC and identified by MS,¹H-NMR and ¹³C-NMR.RESULTS 26 mg luteolin,15 mg 5-hydroxyl-7,4′-dimethoxy flavone and 21 mg 5-hydroxyl-7,3′,4′-trimethoxy flavone with purities of over 98% were obtained from 400 mg crude extract in one-step elution and less than 6 hours.CONCLUSION Three kinds of flavones are all discovered from the plant of Patrinia genius for the first time.The results indicate that HSCCC is a powerful technique of purification for natural products.