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Method for refining salvianolic acid A and protocatechuic aldehyde simultaneously

A technology of protocatechualdehyde and salvianolic acid, which is applied in the field of medicine, can solve the problems of easy emulsification, high solubility in water, and low selectivity of salvianolic acid A extractant, and achieve solvent recovery and regeneration with high interfacial tension , the effect of easy phase separation

Active Publication Date: 2017-08-11
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of this invention is to solve the problems such as low selectivity of salvianolic acid A extractant reported, high solubility in water and easy to produce emulsification phenomenon, a kind of method for refining salvianolic acid A and protocatechualdehyde simultaneously proposed, adopt specific The extraction agent, only by liquid-liquid extraction and refining salvianolic acid A and protocatechualdehyde at the same time

Method used

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  • Method for refining salvianolic acid A and protocatechuic aldehyde simultaneously
  • Method for refining salvianolic acid A and protocatechuic aldehyde simultaneously
  • Method for refining salvianolic acid A and protocatechuic aldehyde simultaneously

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Take 1Kg of Salvia miltiorrhiza, add 6Kg of water, decoct for 120min, then filter to get the filtrate. Add 6Kg of water, decoct for 120min and then filter to get the filtrate. The two filtrates were combined and then concentrated under reduced pressure until the concentrated solution was 1.10 g / mL for use. Take 800g of ethyl acetate and 200g of n-heptane, and mix them to make extractant S1 for later use. Take 999g of ethyl acetate and 1g of n-heptane, and mix them to make extractant S2 for later use.

[0036] Take 200g of extractant S1, extract 100g of Danshen water-extracted concentrate in a separatory funnel, shake fully and let stand to separate phases. After phase separation, extract E1 and raffinate R1 are obtained. Wash the extract E1 twice with 700 mL of water in a separatory funnel to obtain an organic phase O1 after washing. The organic phase O1 was vacuum-dried at low temperature to obtain protocatechualdehyde with a purity of 90.2% and a recovery rate of ...

Embodiment 2

[0039] Take 1Kg of Salvia miltiorrhiza, add 6Kg of water, decoct for 120min, then filter to get the filtrate. Add 6Kg of water, decoct for 120min and then filter to get the filtrate. The two filtrates were combined and then concentrated under reduced pressure until the concentrated solution was 1.08 g / mL for use. Take 200g of n-butanol and 800g of n-pentane, and mix them to make extraction agent S1 for later use. Take 500g of n-butanol and 500g of n-pentane, and mix them to make extractant S2 for later use.

[0040]Take 200g of extractant S1, extract 100g of Danshen water-extracted concentrate in a separatory funnel, shake fully and let stand to separate phases. After phase separation, extract E1 and raffinate R1 are obtained. Wash the extract E1 twice with 600 mL of water in a separatory funnel to obtain an organic phase O1 after washing. The organic phase O1 was vacuum-dried at low temperature to obtain protocatechualdehyde with a purity of 93.6% and a recovery rate of 7...

Embodiment 3

[0043] Take 1Kg of Salvia miltiorrhiza, add 6Kg of water, decoct for 120min, then filter to get the filtrate. Add 6Kg of water, decoct for 120min and then filter to get the filtrate. The two filtrates were combined and then concentrated under reduced pressure until the concentrated solution was 1.15 g / mL for use. Take 300g of methyl isobutyl ketone and 700g of isooctane, and mix them to prepare extractant S1 for use. Take 600g of methyl isobutyl ketone and 400g of isooctane, and mix them to make extractant S2 for later use.

[0044] Take 200g of extractant S1, extract 100g of concentrated salvia miltiorrhiza in a separatory funnel, shake it well, let it stand for phase separation, repeat the extraction three times, and combine the extracts to obtain extract E1 and raffinate R1. Wash the extract E1 twice with 1500 mL of water in a separatory funnel to obtain an organic phase O1 after washing. The organic phase O1 was vacuum-dried at low temperature to obtain protocatechualde...

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Abstract

The invention discloses a method for refining salvianolic acid A and protocatechuic aldehyde simultaneously. The method employs salvia miltiorrhiza water-extracted concentration as a raw material, and prepares salvianolic acid A and protocatechuic aldehyde by an extraction method. The method is characterized by performing extraction through an alkane-containing mixed solvent. Through changing the ratio of alkanes in the mixed solvent, protocatechuic aldehyde is extracted and separated from the salvia miltiorrhiza water-extracted concentrate, and then salvianolic acid A is extracted and separated. Through water-washing and drying the extract, the high-purity salvianolic acid A and protocatechuic aldehyde can be obtained separately. According to the method, the extracting selectivity can be improved by using alkanes as an extracting agent, and the emulsifying chances in extraction are reduced. The salvianolic acid A and protocatechuic aldehyde can be purified at the same time through extraction only; the method uses no complex operation and has the advantages of simple technique, easiness of amplifying, continuous production, low loss of extracting agents, and the like; therefore, the method is suitable for refining salvianolic acid A and protocatechuic aldehyde simultaneously.

Description

technical field [0001] The invention belongs to a separation method in the field of medicine, in particular to a method for simultaneously refining salvianolic acid A and protocatechualdehyde. Background technique [0002] Salvianolic acid A is a significant pharmacologically active ingredient in Salvia miltiorrhiza, which can protect myocardial ischemia, prevent atherosclerosis and embolism, protect cerebral ischemia damage, protect learning and memory damage, prevent Parkinson's disease, prevent and treat tumors, Regulate the immune system, promote bone formation, and protect gastric mucosal damage. Protocatechualdehyde (3,4-dihydroxybenzaldehyde) is another important active ingredient in Salvia miltiorrhiza, which is used as a quantitative detection ingredient in various Danshen preparations. Myocardial ischemia, inhibition of platelet aggregation, repair of damaged venous valves, treatment of varicose veins, and broad-spectrum antibacterial and anti-inflammatory effects...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/48C07C69/732C07C45/78C07C47/565
CPCC07C45/78C07C67/48C07C69/732C07C47/565
Inventor 瞿海斌潘坚扬龚行楚
Owner ZHEJIANG UNIV
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