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Preparation method of protocatechualdehyde

A technology of acidic water and Salvia miltiorrhiza is applied in the preparation of organic compounds, the preparation of carbon-based compounds, chemical instruments and methods, etc., and can solve the problems of high cost, complex method steps, and difficult control.

Inactive Publication Date: 2007-04-25
SHANDONG LUYE PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Yao Junyan etc. extracted with boiling water, then extracted with ether and prepared by thin layer to obtain protocatechualdehyde [Yao Junyan et al., Journal of Nanjing Pharmaceutical University, 1979 (1)]; Chen Zhengxiong extracted Danshen injection with ether, concentrated and separated out protocatechuic aldehyde Aldehydes [Chen Zhengxiong, Gu Wenhua, Huang Huizhu, Pharmaceutical Bulletin, 1981, 16 (9)], but these methods have small preparation amount, high cost, and residual toxicity problems, and are not suitable for large-scale industrial production
Chinese patent application CN97101869 adopts the method of chemical synthesis to prepare protocatechualdehyde, and the steps of this method are complicated and difficult to control
There is no report on the method of preparing high-purity protocatechuic aldehyde by industrial production by extraction method

Method used

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Examples

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Effect test

preparation example 1

[0013] Extract 50 kg of medicinal material Salvia miltiorrhiza with 1200 L of 0.4% sodium hydroxide solution to obtain an extract containing protocatechuic aldehyde; adjust the extract to neutrality with hydrochloric acid, and use an adsorption column filled with weakly alkaline macroporous adsorption resin D301M for adsorption , after the adsorbent is saturated, elute with 50% (V / V) 400L of ethanol solution and 0.4% (m / V) 500L of sodium hydroxide aqueous solution, collect the eluate, concentrate to about 20L, and wash with hydrochloric acid Adjust to a pH value of 2, use an adsorption column filled with a weakly polar adsorbent AB-8 to carry out acidic conditions (pretreatment, the treated resin is eluted with hydrochloric acid solution until the pH value of the eluent is 2) adsorption, and use pure Elute with 800L of water, then use 5% ethanol solution to elute 800L, collect the eluent, concentrate to obtain 2L of concentrated solution; cool, stand still to obtain protocatech...

preparation example 2

[0015] 50 kg of medicinal material Salvia miltiorrhiza was extracted with 1200 L of 0.4% sodium hydroxide solution to obtain an extract containing danshensu; the extract was adjusted to neutrality with hydrochloric acid, and was adsorbed with an adsorption column filled with weakly basic macroporous adsorption resin D301R, and waited for After the adsorbent is saturated, elute with 60% (V / V) 450L of ethanol solution and 0.5% (m / V) 600L of sodium hydroxide aqueous solution, collect the eluate, concentrate to about 10L, and adjust to The pH value is 3, and the adsorption column is filled with weakly polar adsorbent AB-8 for acidic conditions (the treated resin is eluted with hydrochloric acid solution until the pH value of the eluent is 3) adsorption, hydrochloric acid aqueous solution 0.2% (V / V ) 750L elution, then use 10% ethanol solution to elute 500L, collect the eluent, concentrate to obtain 1.5L of concentrated solution, cool, stand still, obtain protocatechualdehyde crysta...

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PUM

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Abstract

The invention discloses a preparing method of protocatechuic acid, which comprises the following steps: adsorbing extracted salvia miltiorrhizae alkaline through weak base resin; adjusting pH value of eluent at 1-4; eluting through pure water or acid first and low-density alcohol then; collects alcohol cleaning solution; condensing; cooling; fitting for large scale of industrial manufacturing.

Description

technical field [0001] The invention relates to a preparation method of protocatechualdehyde. Background technique [0002] Protocatechuic aldehyde is a water-soluble component of the traditional Chinese medicine Danshen (Salvia miltiorrhiza Bge.), which has the effect of significantly dilating coronary arteries and increasing coronary flow [Liu Yan, et al., Quality Evaluation Methods for Salvia Miltiorrhiza and Its Preparations, Chinese Journal of Traditional Chinese Medicine, 1990, 15(3)], its chemical name is 3,4-dihydroxybenzaldehyde. [0003] Most of the methods for preparing high-purity protocatechualdehyde in the literature are extracted with organic solvents. Yao Junyan et al. extracted with boiling water, then extracted with ether and prepared by thin layer to obtain protocatechualdehyde [Yao Junyan et al., Journal of Nanjing Pharmaceutical University, 1979 (1)]; Chen Zhengxiong extracted Danshen injection with ether, concentrated and separated out protocatechuic a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/00C07C47/565
Inventor 岳喜典曲桂武
Owner SHANDONG LUYE PHARMA CO LTD
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