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Preparation of Salvianolic Acid A by the Degradation Reaction of Salvianolic Acid B in Subcritical Water Integrated With pH-zone-refining Counter-Current Chromatography

Preparation of Salvianolic Acid A by the Degradation Reaction of Salvianolic Acid B in Subcritical Water Integrated With pH-zone-refining Counter-Current Chromatography

Huaizhi Li, Yan Cheng, Hongjing Dong, Xiao Wang, Jia Li, Qianshan Gao

J Chromatogr A. 2016 Oct 14;1468:42-48.

PMID: 27670752

Abstract:

Salvianolic acid A is the major bioactive compound in Danshen, however, due to the chemical instability and low content in Danshen, it is difficult to extract amount of salvianolic acid A. Therefore, this study was to establish an effective strategy for obtaining adequate amount of salvianolic acid A, subcritical water extraction was used to degrade salvianolic acid B and prepare salvianolic acid A. Different reaction conditions including temperature, time, concentration and pH value in subcritical water were investigated. Under 40mg/mL of reactant concentration, 180°C of temperature, 4.0 of pH value and 60min of reaction time, the highest yield rate of salvianolic acid A reached 34.86%. Then, the degradation products were successfully separated by pH-zone-refining counter-current chromatography with the solvent system Pet-EtAc-n-BuOH-H2O (2:3:1:9, v/v), where 10mM TFA was added in stationary phase and 10mM NH3·H2O in mobile phase. As a result, a total of 227.3mg of salvianolic acid A at 98.2% purity, 38.9mg of danshensu at 99.3% purity, 9.5mg of salvianolic acid D at 92.7% purity, and 32.8mg of protocatechuic aldehyde at 93.1% purity were obtained from 1.2g degradation products of salvianolic acid B by one-step purification. The results demonstrated that the combinative application of subcritical water and pH-zone-refining counter-current chromatography is a potential technique for the preparative separation of salvianolic acid A from salvianolic acid B.

Chemicals Related in the Paper:

Catalog Number	Product Name	Structure	CAS Number	Price
AP142998478	Salvianolic acid D		142998-47-8	Price

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