TBE-200V 高速逆流色谱仪

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。

摘要: 高速逆流色谱分离生物碱是目前中药有效成分分离中的热点,本文用制备型高速逆流色谱,从黄连、黄柏、十大功劳和金果榄等四种中药中分离出了几种小檗碱类生物碱.分离的基本方法都是把中药材进行粉碎,然后用工业酒精浸泡,滤液浓缩后用浓盐酸酸化过滤,滤液用氢氧化钠碱化至pH=10后用氯仿萃取,氯仿萃取液浓缩所得浸膏作为分离的样品.分离的溶剂体系主要由四氯化碳、氯仿、甲醇和稀盐酸以不同的体积比组成,分离条件是流速为2mL/min,转速为800r/min,进样量为200mg.分离所得组分用标准品进行对照,确定结构.

摘 要：用国产高速逆流色谱(HSCCC) 分离纯化中草药———丹参,选用正己烷-乙醇-水体系,固定相保留率达到78.8 %。采用分步洗脱,3 个产地丹参各分离得到12 个洗脱组分,经高效液相色谱仪和紫外光谱仪检测证明3 张HSCCC洗脱图谱中对应洗脱峰为同一组分。HSCCC 洗脱图谱不包含非共有峰,并且对应洗脱峰保留时间的相对标准偏差RSD < 3 % ,符合国家标准关于制订指纹图谱方法学考察资料的技术参数。因此,HSCCC 作为制订指纹图谱的方法之一具有可行性.

摘要:应用高速逆流色谱法对环抱菌素的分离纯化进行研究,选择石油醚-丙酮-水(3:3:2,V/V)为两相体系,计算环抱菌A,B,C,D在两相体系中的分配系数,以上相为固相,下相为流动相进行高速逆流色谱分离纯化,高效液相色谱法测定单组分纯度。实验结果表明一次高速逆流色谱即可将环抱菌素粗品分离纯化,得到纯度98.5%以上的环抱菌素A,B,C,D单组分,收率达85%以上。