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Preparation method for high-purity baicalin

A baicalin, high-purity technology, applied in the field of preparation of high-purity baicalin, can solve the problems of complex solvent residue removal process, low resin adsorption efficiency, yield and purity impact, etc., to achieve clinical application and convenience for follow-up The effect of treatment and avoiding secondary hydrolysis

Active Publication Date: 2016-05-11
SHANDONG ANALYSIS & TEST CENT
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  • Summary
  • Abstract
  • Description
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Problems solved by technology

[0012] The preparation technology of above-mentioned baicalin generally has the following disadvantages: (1) the combined application of strong acid and strong alkali and heating conditions easily causes further hydrolysis of baicalin in the production process, and the yield and purity are all affected
(2) The baicalin precipitate formed in water and alcohol is a very fine amorphous crystal, which is easy to form a paste with the solvent, and the filtration operation is very cumbersome
(3) The adsorption efficiency of the resin is not high, and it usually needs to be treated with solvent crystallization, which is not easy to achieve large-scale production
(4) The processing scale is small, not suitable for the requirements of industrial production
[0013] The applicant’s previous Chinese patent application CN104650165A disclosed a method for dissolving baicalin by adding an amide solvent, diluting it with alcohols, and obtaining high-purity baicalin through two crystal transformations. Although it does not need to use resin adsorption, it can achieve large-scale However, it still needs two crystallization transformations and multiple filtration operations to obtain high-purity baicalin, and the amide solvent in the pharmaceutical industry is usually a high-boiling-point second-class solvent, and the solvent residue removal process is more complicated

Method used

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  • Preparation method for high-purity baicalin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Embodiment one: the preparation of high-purity baicalin

[0044]1) Take 100.0 g of crude baicalin (content 83%), add it to a mixed solvent of 110 g of dimethyl sulfoxide (DMSO) and 200 g of methanol, stir and heat to 60° C. to dissolve, and obtain a baicalin solution;

[0045] 2) filter to remove insoluble impurities;

[0046] 3) Add 1000 g of methanol to the filtrate.

[0047] 4) Stir and heat to reflux to generate a yellow precipitate, and keep warm for 1 hour;

[0048] 5) cooling, filtering, washing with methanol, and drying to obtain 75.2 g of the product.

[0049] The HPLC determination method of baicalin is: isocratic elution, detection wavelength 280nm, column temperature 25°C, mobile phase: methanol-0.2% phosphoric acid aqueous solution (47:53), octadecylsilane bonded silica gel as filler. The HPLC determination method is detected according to the baicalin standard (standard number WS-10001-(HD-0989)-2002), which is sourced from "National Standards for Local ...

Embodiment 2

[0051] Embodiment two: the preparation of high-purity baicalin

[0052] 1) Take 100.0 g of crude baicalin (content 83%), add it into a mixed solvent of 100 g of dimethyl sulfoxide (DMSO) and 50 g of ethanol, stir and heat to 70° C. to dissolve, and obtain a baicalin solution;

[0053] 2) filter to remove insoluble impurities;

[0054] 3) Add 400 g of ethanol to the filtrate.

[0055] 4) Stir and heat to reflux to generate a yellow precipitate and keep it warm for 1.5 hours;

[0056] 5) Cool, filter, wash with methanol, and dry to obtain 78.5 g of the product. .

[0057] The assay method of baicalin refers to Example 1, and its liquid phase spectrum is shown in figure 2 , HPLC assay content: 98.7%.

Embodiment 3

[0058] Embodiment three: the preparation of high-purity baicalin

[0059] 1) Take 100.0 g of crude baicalin (content 83%), add it to a mixed solvent of 250 g of dimethyl sulfoxide (DMSO) and 150 g of isopropanol, stir and heat to 90° C. to dissolve, and obtain a baicalin solution;

[0060] 2) filter to remove insoluble impurities;

[0061] 3) Add isopropanol 800g again in the filtrate.

[0062] 4) Stir and heat to reflux to generate a yellow precipitate and keep it warm for 0.5 hours;

[0063] 5) Cool, filter, wash with ethanol, and dry to obtain 78.9 g of the product.

[0064] The assay method of baicalin refers to Example 1, and its liquid phase spectrum is shown in image 3 , HPLC assay content: 97.6%.

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Abstract

The invention discloses a preparation method for high-purity baicalin and belongs to the technical field of natural product chemistry. The preparation method includes the following steps that 1, a baicalin crude product is taken and added into mixed solvent of dimethyl sulfoxide and lower alcohol, and the mixture is stirred and heated to 30 DEG C-70 DEG C to be dissolved to obtain a baicalin solution, wherein the mass ratio of the baicalin crude product to dimethyl sulfoxide to lower alcohol is 1:(0.8-3):(0-2) according to the addition amount; 2, filtering is performed to remove insoluble impurities and collect filtrate; 3, lower alcohol is added into the filtrate in the step2, the mass ratio of lower alcohol to the baicalin crude product is (3-10):1 according to the addition amount of lower alcohol, the mixture is constantly stirred and heated to 50 DEG C-90 DEG C to generate yellow sediment, and temperature is kept for 0.5-3 hours; 4, cooling, filtering, lower alcohol washing and lower alcohol drying are performed to obtain yellow powder which is high-purity baicalin. Operation conditions are mild; because no high-boiling-point second-class solvent is used, follow-up treatment of residual solvent is facilitated; the preparation method is suitable for large-scale production.

Description

technical field [0001] The invention relates to the technical field of natural product chemistry, in particular to a preparation method of high-purity baicalin. Background technique [0002] Baicalin is the main medicinal ingredient of commonly used traditional Chinese medicine Scutellaria baicalensis. It has anti-inflammatory, anti-virus, anti-tumor, anti-allergic, blood-lipidemic and blood pressure-lowering activities. It also has anti-oxidation, scavenging oxygen free radicals, and can inhibit the formation of melanin. . High-purity baicalin is clinically used for the treatment of pneumonia, hepatitis, infection and other diseases, and is also often used as a raw material for health care products and beauty cosmetics. [0003] Baicalin is a flavonoid derivative with a glucuronic acid structure, which can be hydrolyzed to produce baicalein and glucuronic acid. The molecular structure of baicalin is as follows: [0004] [0005] The pKa value of baicalin is 5.047, whi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/06
CPCC07H1/06C07H17/07
Inventor 高乾善王晓纪文华赵恒强王岱杰耿岩玲宋祥云
Owner SHANDONG ANALYSIS & TEST CENT
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