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Method for preparing high-purity protocatechualdehyde from salvia miltiorrhiza

A protocatechuic aldehyde, high-purity technology, applied in the field of medicine, can solve the problems of inability to achieve high purity, no process investigation, low catechuic aldehyde purity, etc., and achieve the effects of low cost of materials, less impurities, and high purity.

Active Publication Date: 2011-11-16
TIANJIN TASLY PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yao Junyan and Chen Zhengxiong obtained a small amount of protocatechualdehyde from Danshen and Danshen preparations by ether extraction method for testing, but because there is no systematic process investigation, it cannot be called a preparation method
Chinese patent 1161954 discloses a method for preparing protocatechuic aldehyde from Salvia miltiorrhiza, which is processed by simple two-step chromatography, which cannot meet the high purity requirement
Protocatechuic aldehyde obtained by existing preparation methods has low purity, many impurities, and poor stability, and there are many shortcomings, which have not been solved well for a long time.

Method used

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  • Method for preparing high-purity protocatechualdehyde from salvia miltiorrhiza
  • Method for preparing high-purity protocatechualdehyde from salvia miltiorrhiza
  • Method for preparing high-purity protocatechualdehyde from salvia miltiorrhiza

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] Embodiment 1: the preparation of high-purity protocatechualdehyde, its process step is:

[0082] 1. Preparation of Salvia Miltiorrhiza Extract

[0083] 8kg Danshen decoction pieces, decoct with 6 times the amount of alkaline water (0.45% sodium bicarbonate) for 2 hours, filter, decoct the dregs with 5 times the amount of water for 1 hour, filter, combine the extracts, and concentrate to RD1.20 (80°C) , precipitated to 70% with alcohol, and concentrated the supernatant to RD1.35 (60° C.) to obtain 0.46 kg of Danshen extract.

[0084] Wherein, it needs soaking for 30-60 minutes before adding alkali solution and heating for extraction.

[0085] 2. Chromatography removes relatively small polar Salvia components ( figure 1 )

[0086] Add water to dissolve the salvia miltiorrhiza extract to 0.8 L (0.1 times of the salvia miltiorrhiza decoction pieces), add it into a 3 kg AB-8 macroporous adsorption resin column, elute with water, and collect 18 L of eluate.

[0087] 3. Ch...

Embodiment 2

[0097] Basically the same as Example 1, except that the eluate in step 6 was concentrated under reduced pressure, extracted three times with an equal volume of ethyl acetate, combined, concentrated to dryness under reduced pressure, and obtained.

Embodiment 3

[0099] 1. Preparation of Salvia Miltiorrhiza Extract

[0100] 60kg Danshen decoction pieces, decoct twice (2h, 1h) with 6 times the amount of alkaline water (0.45% sodium bicarbonate) and 5 times the amount of water respectively, filter, combine the extracts, concentrate to RD1.20 (80°C), alcohol sink to 70%, take the supernatant and concentrate to RD1.35 (60°C), to obtain 3.6kg of Danshen extract.

[0101] 3. Chromatography removes relatively small polar components of Salvia miltiorrhiza

[0102] Salvia miltiorrhiza extract was dissolved in water to 6L, added to a 20kg AB-8 macroporous adsorption resin column, eluted with water, and 140L of eluate was collected.

[0103] 3. Separation of protocatechualdehyde by chromatography

[0104] The eluate was adjusted to pH 3.0 with acid, added to AB-8 macroporous adsorption resin filled with 20kg, eluted with acid water with pH 2.5-3.5, collected 180L eluate, discarded, and continued to connect 230L eluent.

[0105] 4. Deacidifica...

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Abstract

The invention belongs to field of medicines and relates to a method for preparing high-purity protocatechualdehyde. The preparation method comprises the following steps: 1, preparing salvia miltiorrhiza extract by alkaline extraction and alcohol precipitation; 2, removing salvia miltiorrhiza components with relatively weak polarity by chromatography; 3, separating protocatechualdehyde by chromatography; 4, removing acid and decoloring; 5, refining and purifying; and 6, drying.

Description

technical field [0001] The invention belongs to the field of medicine, and in particular relates to a preparation method for extracting high-purity protocatechuic aldehyde from traditional Chinese medicine salvia miltiorrhiza. technical background [0002] Protocatechuic aldehyde, also known as Guanxinning, is one of the water-soluble active components of Salvia miltiorrhiza. Its structure is: [0003] [0004] Protocatechualdehyde [0005] Its physical properties: light beige needle crystal (water or toluene) or off-white powder, twin crystal. Melting point (m.p.) 153°C ~ 154°C. K=2.8×10-8 (25°C). Soluble in ethanol, acetone, ethyl acetate, ether and hot water, soluble in cold water, insoluble in benzene and chloroform. Solubility in water (g / 100ml): 5 (20°C); 33 (99°C); Solubility in ethanol: 79 (78°C). It has hygroscopicity and is easy to oxidize and change color in water. [0006] Modern pharmacological studies have shown that: Protocatechuic aldehyde has the fo...

Claims

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Application Information

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IPC IPC(8): C07C47/565C07C45/78
Inventor 靳元鹏罗学军陈晓鹏周水平
Owner TIANJIN TASLY PHARMA CO LTD
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