Effect of inorganic salt on partition of high‐polarity parishins in two‐phase solvent systems and separation by high‐speed counter‐current chromatography from Gastrodia elata Blume

Abstract

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.

Biphasic alcoholysis coupled with high‐speed countercurrent chromatography for high performance on separating phorbol from Croton tiglium Linn extracts

“…Besides, the presence of surfactants in crude pgrobol sample may result in the formation of emulsion in the solvent system. Fortunately, the lower phase composed of inorganic salts is considered as a solution to solve these problems [44,45].…”

Identification of Novel Parishin Compounds from the Twig of Maclura tricuspidata and Comparative Analysis of Parishin Derivatives in Different Parts

“…Compound 7 (peak no. 7 in Figure 3E) was isolated as a white amorphous powder from the water fraction by repeated silica gel and Toyopearl HW-40S column chromatography and the molecular formula was determined to be C 19 [44,45], except one carboxyl group in the citric acid moiety was substituted by a methyl group (δ C 27.7; δ H 1.31, 3H, s, C-6). The NMR spectra of this compound showed one oxygenated-olefin quaternary (δ C 131.4, C-1 ), four olefin methine [(δ C 117.7; δ H 7.08, 2H, d, J = 8.4 Hz, C-3 , 5 ) and (δ C 130.9; δ H 7.30, 2H, d, J = 8.4 Hz, C-2 , 6 )], one olefin quaternary (δ C 159.0, C-4 ) and one oxygenated-methylene (δ C 66.9; δ H 5.05, 2H, s, C-7 ) signals, due to the presence of 4-HBA as an aglycone moiety.…”

Separation and purification of benzylester glucosides and derivatives from tubers of Gymnadenia conopsea (L.) R. Br. by linear gradient counter‐current chromatography combined with elution‐extrusion mode

“…Recently, many gradient elution CCC modes were established with the changing of CCC mobile phase types, such as changing mobile phase ratio (stepwise solvent gradients mode), pH value (pH-zone refining CCC mode), salt concentration (salting-out mode), biphasic linear gradients (linear gradient CCC mode, LGCCC) and altered elution phase (elution-extrusion CCC mode, EECCC) [18,[20][21][22]. Among them, LGCCC and elution-extrusion mode were smart and convenient for the separation of complex mixtures in natural products.…”