An extracting, separating and purifying method of salvianolic acid A and a preparing method of salvianolic acid salts

A technology for separation and purification of salvianolic acid, which is applied in the field of medicine, can solve the problems of extremely high requirements for purified samples, low yield of salvianolic acid A, and high cost of reversed-phase silica gel, and achieves time-saving purification methods, low cost, and high production costs. low effect

Inactive Publication Date: 2016-04-27
SHANDONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Chinese patent document CN1384090A discloses a method for extracting salvianolic acid from the traditional Chinese medicine Salvia miltiorrhiza and a preparation method of the preparation thereof, and the preparation method of the salvianolic acid obtained by the method of the present invention and the preparation thereof are used in the prevention and treatment of cardiovascular and cerebrovascular diseases, and the prevention and treatment of senile dementia. and the application of drugs such as the treatment of learning and memory decline caused by cerebral ischemia; however, this process increases alcohol precipitation and causes 30% loss of phenolic acids
Chinese patent document CN1513848A discloses a method for extracting the components of salvianolic acid from traditional Chinese medicine and its freeze-dried powder injection for the prevention and treatment of diseases such as liver injury and liver fibrosis; Salvianolic acid A was prepared by acid and organic solvent extraction and then reversed-phase column chromatography. It was purified by reversed-phase silica gel, which had extremely high requirements for the purified sample, and the cost of reversed-phase silica gel was also high. The content of salvianolic acid A in medicinal materials was low. , or even none, so the yield of salvianolic acid A is low and the production cost is high

Method used

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  • An extracting, separating and purifying method of salvianolic acid A and a preparing method of salvianolic acid salts
  • An extracting, separating and purifying method of salvianolic acid A and a preparing method of salvianolic acid salts
  • An extracting, separating and purifying method of salvianolic acid A and a preparing method of salvianolic acid salts

Examples

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Effect test

Embodiment 1

[0057] A method for purifying, separating and purifying salvianolic acid A, the steps are as follows:

[0058] With reference to the method disclosed in Chinese patent document CN102793745A (Application No.: 201210334295.7), Salvia miltiorrhiza is pretreated; the HPLC figure of Salvia miltiorrhiza after treatment is as follows figure 1 shown.

[0059] (1) Solvent extraction: take the processed Salvia miltiorrhiza as raw material, get 500g, add 12 times the amount of 75wt% ethanol solution as the extraction solvent and carry out ultrasonic extraction, the ultrasonic temperature is 30 ° C, the number of times of extraction is 3 times, each 30 minutes, Remove the dregs and combine the filtrates.

[0060] (2) Solvent extraction: the above-mentioned filtrate is concentrated under reduced pressure to no ethanol, diluted with water, the amount of water added is 2 times the weight of the concentrated solution, and then extracted twice with equal volume of dichloromethane to degrease,...

Embodiment 2

[0069] A method for purifying, separating and purifying salvianolic acid A, the steps are as follows:

[0070] Pretreatment of Salvia miltiorrhiza with reference to the method disclosed in Chinese patent document CN102793745A (application number: 201210334295.7);

[0071] (1) Solvent extraction: take the processed salvia miltiorrhiza as raw material, get 500g, add 8 times the amount of 75wt% ethanol solution as the extraction solvent and carry out ultrasonic extraction, the ultrasonic temperature is 30 ° C, the number of times of extraction is 4 times, each 30 minutes, remove dregs, combined filtrate.

[0072] (2) Solvent extraction: Concentrate the above filtrate under reduced pressure to no ethanol, dilute with water, the amount of water added is twice the weight of the concentrated solution, and then extract and degrease with an equal volume of dichloromethane until the dichloromethane layer is light in color, discard The dichloromethane layer was adjusted to pH=1-2 with 2...

Embodiment 3

[0081] It is basically the same as Example 1, except that step (1) adds 10 times the amount of 75wt% ethanol solution as the extraction solvent for ultrasonic extraction, the ultrasonic temperature is 50°C, and the extraction times are 3 times, each time 40 minutes, to obtain salvianol Acid A was 92.4% pure.

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Abstract

The invention relates to an extracting, separating and purifying method of salvianolic acid A and a preparing method of salvianolic acid A salts. The extracting, separating and purifying method adopts salvia miltiorrhiza bunge var.alha or danshen root as a raw material and includes steps of solvent extraction, solvent extraction, concentration for drying, separation, purification, MCI column separation, crystallization and recrystallization to obtain the salvianolic acid A. Compared with macroporous resin columns, polyamide column chromatography adopted by the extracting, separating and purifying method can purify phenolic acid components more effectively and has better purification effects. A salvianolic acid A magnesium salt complexing process is adopted, and therefore chromatographic processes using macroporous resin or polyamide column chromatography can be omitted, and the purifying method is simpler, more time-saving and lower in cost. The preparing method of the salvianolic acid A magnesium salt is simple and suitable for large-scale production. A salvianolic acid A ammonium salt is a novel salvianolic acid A salt compound.

Description

technical field [0001] The invention relates to a method for extracting, separating and purifying salvianolic acid A, an active ingredient of medicine, and a method for preparing a salt thereof, belonging to the technical field of medicine. Background technique [0002] Danshen is one of the most commonly used medicinal materials for the treatment of cardiovascular and cerebrovascular diseases such as angina pectoris, hypertension, coronary heart disease and stroke. Salviamiltiorrhiza Bungevaralba is a variant of Salvia miltiorrhiza Bungevaralba, which is mainly distributed in Shandong Province, where it is often used as Salvia miltiorrhiza. Studies have shown that not only the chemical composition of salvia miltiorrhiza is basically the same as that of salvia miltiorrhiza, but the salvianolic acid components are mainly salvianolic acid B, and the content of salvianolic acid A is very small. [0003] Du Guanhua and others conducted a lot of research on the activity of salvi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/48C07C67/56C07C67/28C07C69/732
CPCC07C67/28C07C67/48C07C67/56C07C69/732
Inventor 孙隆儒张愉朱炳洁季梅
Owner SHANDONG UNIV
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