Method for preparing tanshinone IIA and dihydrotanshinone I by adopting medium/high-pressure preparation liquid-phase method

A technology for dihydrotanshinone and liquid phase preparation, which is applied in the fields of steroids and organic chemistry, and can solve problems such as pollution, traditional Chinese medicine resource waste environment, and low utilization efficiency of salvia miltiorrhiza resource materials, achieving good technical effects and reasonable process design Effect

Active Publication Date: 2017-06-13
NANJING UNIVERSITY OF TRADITIONAL CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, a large amount of solid waste of Danshen is generated in the production process of Danshen injection, which leads to low utilization efficiency of Danshen resource substances, and causes serious waste of traditional Chinese medicine resources and environmental pollution.

Method used

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  • Method for preparing tanshinone IIA and dihydrotanshinone I by adopting medium/high-pressure preparation liquid-phase method
  • Method for preparing tanshinone IIA and dihydrotanshinone I by adopting medium/high-pressure preparation liquid-phase method
  • Method for preparing tanshinone IIA and dihydrotanshinone I by adopting medium/high-pressure preparation liquid-phase method

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Experimental program
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Effect test

Embodiment 1

[0029] The method for preparing tanshinone IIA and dihydrotanshinone I by medium and high pressure preparation liquid phase method comprises the following steps:

[0030] Step A: Extract the dregs of salvia miltiorrhiza with water, dry, crush and sieve to obtain salvia miltiorrhiza powder, add 8 times the amount of ethanol solution with a volume concentration of 70, carry out reflux extraction twice, each time for 2 hours, combine the extracts and concentrate to obtain salvia miltiorrhiza Alcoholic extract extract.

[0031] Step B: Take 100g of the alcoholic extract of Salvia miltiorrhiza, add 1000mL of pure water to dissolve, extract with petroleum ether and ethyl acetate respectively, repeat the extraction three times, combine the extracts of the ethyl acetate part, concentrate under reduced pressure, and obtain the concentrated part of the ethyl acetate liquid.

[0032] Step C: Weigh the concentrated solution of the ethyl acetate part to be separated and add double the amo...

Embodiment 2

[0036] The method for preparing tanshinone IIA and dihydrotanshinone I by medium and high pressure preparation liquid phase method comprises the following steps:

[0037] Step A: extract the dregs of salvia miltiorrhiza with water, dry, crush salvia miltiorrhiza and sieve to obtain salvia miltiorrhiza powder, add 10 times the amount of 80% ethanol solution, carry out reflux extraction twice, each time for 2 hours, combine the extracts and concentrate Obtain the salvia miltiorrhiza alcoholic extract extract.

[0038] Step B: Take 300g of the alcoholic extract of Danshen medicinal dregs, add 3000mL of pure water to dissolve, extract with petroleum ether and ethyl acetate respectively, repeat the extraction 3 times, combine the extracts from ethyl acetate, concentrate under reduced pressure, and obtain ethyl acetate Ester site concentrate.

[0039] Step C: Weigh the concentrated solution of the ethyl acetate part of the sample to be separated and add double the amount of silica ...

Embodiment 3

[0043] The method for preparing tanshinone IIA and dihydrotanshinone I by medium and high pressure preparation liquid phase method comprises the following steps:

[0044] Step A: Extract the dregs of salvia miltiorrhiza with water, dry, crush salvia miltiorrhiza and sieve to obtain salvia miltiorrhiza powder, add 12 times the amount of ethanol solution with 90% volume concentration, carry out reflux extraction twice, each time for 2 hours, combine the extracts and concentrate Obtain the salvia miltiorrhiza alcoholic extract extract.

[0045] Step B: Take 200g of the alcoholic extract of Danshen dregs, add 2000mL of pure water to dissolve, extract with petroleum ether and ethyl acetate respectively, repeat the extraction three times, combine the extracts from the ethyl acetate parts, concentrate under reduced pressure, and obtain ethyl acetate Site concentrate.

[0046] Step C: Weigh the concentrated solution of the ethyl acetate part of the sample to be separated and add doub...

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Abstract

The invention discloses a method for preparing tanshinone IIA and dihydrotanshinone I by adopting a medium / high-pressure preparation liquid-phase method. The method comprises the following steps: (1) drying the salviae miltiorrhizae dreg after aqueous extraction, crushing and concentrating with ethanol, thereby acquiring salviae miltiorrhizae alcohol extract; (2) extracting the extract with petroleum ether and ethyl acetate, taking the part extracted with ethyl acetate and concentrating; (3) adopting medium pressure preparation liquid phase, thereby acquiring a total tanshinone crude extract; (4) adopting UPLC analysis and then merging tanshinone IIA and dihydrotanshinone I; (5) performing high pressure preparation liquid phase separation, thereby acquiring tanshinone IIA and dihydrotanshinone I monomeric compounds. According to the invention, the medium / high-pressure preparation liquid-phase combined technique is adopted for efficiently and quickly separating and purifying high-purity tanshinone IIA and dihydrotanshinone I compound from the salviae miltiorrhizae dreg; the waste resources can be fully utilized; the method has environmental protection significance and economic value.

Description

technical field [0001] The invention belongs to the field of traditional Chinese medicine phytochemistry, and specifically relates to a method for preparing monomeric compounds of tanshinone IIA and dihydrotanshinone I through liquid phase extraction and purification by high pressure. Background technique [0002] Danshen (Salvia miltiorrhiza Bge.) belongs to the labiatae plant, mainly produced in Hebei, Anhui, Jiangsu, Sichuan and other places. It was first recorded in "Shen Nong's Materia Medica". , Qingxin Chufan and other effects. The chemical composition of Danshen is divided into two parts: fat-soluble and water-soluble. Tanshinone (tanshinone, Tsn) is a fat-soluble abietane diterpenoid compound in Danshen, also known as total tanshinone, which has a wide range of pharmacological effects and is recognized by medical scientists. highly anticipated. Fat-soluble tanshinone compounds have a wide range of pharmacological effects and clinical applications. Its chemical st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J73/00
CPCC07J73/003
Inventor 宿树兰段金廒钱大玮郭盛戴新新
Owner NANJING UNIVERSITY OF TRADITIONAL CHINESE MEDICINE
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