Separation and purification method of salvianolic acid B and preparation method of salvianolic acid B magnesium salt

A technology for separation and purification of salvianolic acid, applied in the field of separation and purification of salvianolic acid B, can solve the problems of limited use of high-speed countercurrent chromatography, cumbersome operation process, complicated process, etc., and achieve time-saving purification methods, high purity, and purification methods simple and effective

Inactive Publication Date: 2016-04-13
SHANDONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above method uses silica gel column chromatography to separate and purify salvianolic acid B, and the obtained salvianolic acid B has a purity of 50%-96%; however, the process is complicated, the dead adsorption is large, and the operation process is cumbersome, so it is difficult to expand to production
XiaoWang et al. described in Journal of Separation Science 2007, 30, 3214-3217 the process of using high-speed countercurrent chromatography to separate and purify salvianolic acid B, showing that pH gradient countercurrent chromatography can purify salvianolic acid B to 94.1%, and may be applied to large-scale production; but , the use of high-speed countercurrent chromatography has certain limitations

Method used

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  • Separation and purification method of salvianolic acid B and preparation method of salvianolic acid B magnesium salt
  • Separation and purification method of salvianolic acid B and preparation method of salvianolic acid B magnesium salt
  • Separation and purification method of salvianolic acid B and preparation method of salvianolic acid B magnesium salt

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1: the preparation of high-purity salvianolic acid A

[0039] (1) Extraction of salvianolic acid B: Take about 500g of salvia miltiorrhiza medicinal material powder, add 75wt% ethanol, the mass ratio of salvia miltiorrhiza medicinal material powder to ethanol is 1:12g / mL; ultrasonic extraction 2 times, 30 minutes each time, filter , combined the filtrates, concentrated under reduced pressure, added an appropriate amount of water to the concentrated solution, extracted an equal volume of dichloromethane to remove impurities, adjusted the pH of the aqueous layer to 2 with 2.5N hydrochloric acid, and extracted twice with an equal volume of ethyl acetate. The ethyl acetate extract was concentrated under reduced pressure to obtain the crude extract of salvianolic acid B.

[0040] (2) Magnesium salt complexation purification: NaHCO 3 with MgCl 2Add the solution with a molar ratio of 2:1 into the crude extraction of salvianolic acid B to dissolve it, extract twice...

Embodiment 2

[0045] Embodiment 2: preparation of salvianolic acid B magnesium salt

[0046] Take MgCl 2 Soluble in distilled water, prepared to a concentration of 1wt% MgCl 2 aqueous solution, then dropwise add 1wt% NaOH aqueous solution until no white precipitate is generated, filter the precipitate, wash the precipitate with distilled water until neutral; take Mg(OH) 2 Add water, pass CO 2 60-90min until the solution is clear, and ultrasonic for 10min to remove excess CO in the solution 2 , the solution is filtered to remove insoluble particles, and the magnesium bicarbonate solution is obtained; the magnesium bicarbonate solution must be prepared immediately after use.

[0047] Add 20 mg of the 98% salvianolic acid B sample prepared in Example 1 into the freshly prepared magnesium bicarbonate solution, and shake to dissolve it. Extract with an equal volume of ethyl acetate, combine the extracts, concentrate under reduced pressure and evaporate to dryness to obtain high-purity salvia...

Embodiment 3

[0048] Embodiment 3: preparation of salvianolic acid B magnesium salt

[0049] Take MgCl 2 Soluble in distilled water, formulated to a concentration of 0.05wt% MgCl 2 Aqueous solution; The 98% salvianolic acid B sample 20mg that embodiment 1 prepares joins MgCl 2 In aqueous solution, stirring at room temperature, NaHCO was added dropwise 3 Aqueous solution; after the dropwise addition, filter with suction and freeze-dry to obtain salvianolic acid B magnesium salt complex.

[0050] The MgCl 2 MgCl contained in the solution 2 The ratio of the number of moles to the number of moles of salvianolic acid B is 1:2. Among them, the NaHCO 3 NaHCO contained in the solution 3 The molar ratio of the moles of salvianolic acid B and salvianolic acid B is 1:1.

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Abstract

The invention relates to a separation and purification method of salvianolic acid B and a preparation method of a salvianolic acid B magnesium salt. The separation and purification method of the salvianolic acid B comprises taking a medicinal material of danshen root or white flower danshen as a raw material, and carrying out the steps of solvent extraction, separation and purification through a magnesium salt complexing method, MCI column purification, crystallization and recrystallization. According to the methods provided by the invention, a salvianolic acid B magnesium salt complexing method is adopted, so that a chromatography process with macroporous adsorption resin or polyamide column chromatography can be saved, the purification method is simpler and more time-saving, and the cost is lower. The preparation method of the salvianolic acid B magnesium salt is simple, and is low in cost, high in yield, and high in purity which can reach 98%, so that the preparation method is more suitable for mass production.

Description

technical field [0001] The invention relates to a method for separating and purifying salvianolic acid B from extracts of salvia miltiorrhiza or salvia miltiorrhiza and a preparation method for its magnesium salt. Background technique [0002] The traditional Chinese medicine Salvia miltiorrhiza has the effects of promoting blood circulation and removing blood stasis, cooling blood and eliminating carbuncle, clearing heart and eliminating troubles. Modern pharmacological studies have shown that Danshen can dilate coronary arteries, increase blood flow, resist myocardial ischemia, improve microcirculation, reduce myocardial oxygen consumption, improve heart function, lower blood pressure, lower blood fat, anticoagulant, antithrombotic, antioxidant, Liver protection and many other effects. [0003] Salvianolic acid B is one of the main water-soluble components of Danshen. Pharmacological studies have shown that salvianolic acid B has strong pharmacological effects in scaveng...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/86
CPCC07D307/86
Inventor 孙隆儒张紫茹张愉陈奕名季梅
Owner SHANDONG UNIV
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