Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Qilu University of Technology (Shandong Academy of Sciences), Jinan, P. R. China.
Shandong University of Traditional Chinese Medicine, Jinan, P. R. China.
J Sep Sci. 2019 Feb;42(4):871-877. doi: 10.1002/jssc.201801012. Epub 2019 Jan 18.
Parishins are high-polarity and major bioactive constituents in Gastrodia elata Blume. In this study, the effect of several inorganic salts on the partition of parishins in two-phase solvent systems was investigated. Adding ammonium sulfate, which has a higher solubility in water, was found to significantly promote the partition of parishins in the upper organic polar solvents. Based on the results, a two-phase solvent system composed of butyl alcohol/acetonitrile/near-saturated ammonium sulfate solution/water (1.5:0.5:1.2:1, v/v/v/v) was used for the purification of parishins by high-speed counter-current chromatography. Fractions obtained from high-speed counter-current chromatography were subjected to semi-preparative high-performance liquid chromatography to remove salt and impurities. As a result, parishin E (6.0 mg), parishin B (7.8 mg), parishin C (3.2 mg), gastrodin (15.3 mg), and parishin A (7.3 mg) were isolated from water extract of Gastrodia elata Blume (400 mg). These results demonstrated that adding inorganic salt that has high solubility in water to the two-phase solvent system in high-speed counter-current chromatography was a suitable approach for the purification of high-polarity compounds.
天麻素是天麻中的高极性和主要生物活性成分。在本研究中，考察了几种无机盐对两相溶剂系统中天麻素分配的影响。结果发现，添加在水中溶解度更高的硫酸铵可显著促进天麻素在上层有机极性溶剂中的分配。基于这一结果，采用正丁醇/乙腈/近饱和硫酸铵溶液/水（1.5:0.5:1.2:1，v/v/v/v）两相溶剂系统，通过高速逆流色谱法对天麻素进行了纯化。从高速逆流色谱中得到的馏分通过半制备高效液相色谱法去除盐和杂质。结果，从天麻（400mg）的水提取物中分离得到天麻素 E（6.0mg）、天麻素 B（7.8mg）、天麻素 C（3.2mg）、天麻素（15.3mg）和天麻素 A（7.3mg）。这些结果表明，在高速逆流色谱的两相溶剂系统中添加在水中溶解度高的无机盐是一种适用于高极性化合物纯化的方法。
