高速逆流色谱快速分离制备石椒草中高纯度芦丁对照品

Preparative isolation and purification of rutin from Boenninghausenia sessilicarpa Le’ vl by high speed counter-current chromatography

关键词:  芦丁  石椒草  HSCCC  HPLC

Key words:  Boenninghausenla sessilicarpa Le'vl  rutin  High Performance Liquid Chromatography  High speed counter-current chromatography

摘要:

［目的］建立高速逆流色谱法高效、快速分离制备石椒草中芦丁的新方法。［方法］石椒草的乙醇提取物经大孔吸附树脂柱初步分离后，直接进行高速逆流色谱分离，所用两相溶剂体系为乙酸乙酯–正丁醇–水(2∶1∶3, v/v/v) ，上相为固定相，下相为流动相，流速1.5 mL/min，转速830 r/min，检测波长254 nm，所得产物的纯度经HPLC检测，结构经UV和MS鉴定。［结果］经一步分离从200 mg石椒草粗提物中得到纯度高于99％的芦丁，分离时间短于2 h。［结论］由该法制备芦丁简便、快速，所得产物纯度高，适合于芦丁对照品的大规模制备。

Abstract:

［Objective］To develop an effective and rapid method for preparative purification rutin from Boenninghausenla sessilicarpa Le'vl.［Methods］The crude samples after cleaning-up on macroporous resin column chromatograph from raw material treated by ethanol were separated by high speed counter-current chromatography (HSCCC). In the process, the solvent system composed of ethyl acetate-n-butanol-water (2∶1∶3, v/v/v) was selected, and the upper phase was used as the stationary phase, and the lower phase was used as the mobile phase. The obtained fractions were analyzed by HPLC and identified by UV and MS.［Results］Rutin with purity of over 99% was separation from 200 mg of crude sample from Boenninghausenia sessilicarpa Le'vl.［Conclusions］The established protocol is simple, fast, and suitable for large-scale isolation and suitable for separation rutin from medicinal plants.