上海同田生物技术：运用高速逆流色谱从白术分离纯化苍术酮和苍术烯丙酯Ⅲ

Abstract: A preparative high-speed counter-current chromatography (HSCCC) was used to isolate and separate curculigoside and curculigoside B from the famous traditional Chinese medicinal herb Curculigo orchioides. Some parameters including two-phase solvent system, separation temperature,flow rate of the mobile phase and revolution speed of the apparatus were all investigated, and a successfully isolation and purification was achieved at the following conditions: the two-phase solvent system composed of ethyl acetate-ethanol-water at a volume ratio of 5:1:5(v/v/v) was selected and the lower phase of the system was used as the mobile phase at the flow rate of 2.0ml/min, and the isolation temperature and revolution speed were set at 30◦C and 800rpm.The isolation produced a total of 14.5 mg curculigoside B and 72.8 mg curculigoside with purities of 96.5% and 99.4% determined by high performance liquid chromatography (HPLC) from 300 mg crude extract after cleaning-up by D101 macroporous resin,which was necessary for the excellent purification. The recoveries of the two compounds were 91.6% and 92.5%, respectively, and the chemical structure identification was carried out by UV, MS and NMR. This separation method was more effective than some conventional techniques.

Abstract: Preparative high-speed counter-current chromatography (HSCCC), as a continuous liquid–liquid partition chromatography with no solid support matrix, combined with evaporative light scattering detection (ELSD) was employed for systematic separation and purification of non-chromophoric chemical components from Chinese medicinal herb Adenophora tetraphlla (Thunb.), Fisch. Nine compounds, includingα-spinasterol, β-sitosterol, nonacosan-10-ol, 24-methylene cycloartanol, lupenone, 3-O-palmitoyl-β-sitosterol, 3-O-β-d-glucose-β-sitosterol, eicosanoic acid and an unknown compound, were obtained. The compounds were all above 95% determined by high-performance liquid chromatography (HPLC)–ELSD, and their structures were identified by H-NMR and chemical ionization mass spectroscopy (CI-MS). The results demonstrate that HSCCC coupled with ELSD is a feasible and efficient technique for systematic isolation of non-chromophoric components from traditional medicinal herbs.

摘　要: 采用高速逆流色谱法分离纯化丹参水溶性成分丹酚酸类物质,制备丹酚酸B化学对照品。分离采用的溶剂系统为正己烷2乙酸乙酯2水2甲醇(1.5:5:5:1.5),上相做固定相,下相做流动相,流速为1.7mL/min,仪器转速850rpm,进样量80mg,纯度用HPLC 方法测定。结果表明:一次分离可制备63.4mg丹酚酸B,其纯度为98.6%。该方法操作简单,可作为高纯度丹酚酸B化学对照品的制备分离方法。

摘要：用三种方法对荷叶提取物进行分离纯化，结合薄层层析（TLC）和颜色反应，对各自分离组分跟随鉴定。结果表明：高速逆流色谱（HSCCC）分离效果好，Sephadex LH-20柱层析分离效果次之，硅胶柱层析分离效果最差；荷叶提取物经高速逆流色谱分离纯化，可以得到两种黄酮醇类单体。