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Scutellarin purifying method

A technology of scutellarin and a purification method, which is applied in the field of traditional Chinese medicine preparation, can solve the problems of complex purification process and large amount of organic solvent, and achieve the effect of simple technical route, fewer operation steps and increased safety

Inactive Publication Date: 2011-10-26
ZHEJIANG UNIV
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Problems solved by technology

[0005] The present invention aims at the shortcomings of the existing scutellarin purification process complex process and large amount of organic solvents, and proposes a novel purification method for purifying scutellarin, which is realized by the following steps: firstly, at a certain temperature, the scutellarin The crude product is put into a certain amount of solvent, and the pH is adjusted with an alkaline solution until all scutellarin is dissolved in the solution; then crystals are precipitated by evaporation or cooling, filtered, washed, and dried to obtain refined scutellarin salt Intermediate; reselect the solvent, dissolve the crystalline intermediate product in it, add an appropriate acidic solution, adjust the pH of the solution, and convert the scutellarin salt into the form of scutellarin and precipitate it from the solution; then filter and wash , dried to obtain scutellarin crystals

Method used

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Embodiment 1

[0018] Taking by weighing 5.13g content is the scutellarin crude product of 90% (its high-performance liquid chromatogram sees figure 1 ), added to 60mL water, at 50-60°C, adjust the pH to 8.0~9.0 with 5% NaOH to dissolve the sample completely, put the solution at 4°C to cool down and crystallize for 36h, filter, and wash the precipitate with water until the pH is 7.5, dry to obtain 4.40g of the intermediate precipitate, add all the obtained intermediate to 44mL of 10% ethanol aqueous solution, adjust the pH to 8.0~9.0 with 10% KOH solution, dissolve all, and then adjust the pH with 10% HCl or acetic acid solution to 2.5, filter, wash the precipitate with water to pH 6.8-7.5, dry to obtain refined scutellarin 4.10g, its high performance liquid chromatogram see figure 2 . After calculation, the content of scutellarin is 99.8%, and the product yield in the refining process is 88.6%.

Embodiment 2

[0020] Taking by weighing 5.10g content is the scutellarin crude product of 90% (its high performance liquid chromatogram sees figure 1 ), added to 100mL of water, and then processed according to the operation steps of Example 1 to obtain 3.98g of a refined product containing 99.0% scutellarin, and the product yield was 85.8%.

Embodiment 3

[0022] Weigh 5.28g of crude scutellarin with a content of 90%, add it to 75mL of 10% ethanol aqueous solution, and use 10% Na 2 CO 3 Adjust the pH to 8.0~9.0 to dissolve the sample completely, evaporate under vacuum to reduce the volume of the solution by half, then place the concentrated solution at 8°C to cool down and crystallize for 24 hours, filter, wash the precipitate with water until the pH is 7.5, and dry to obtain Scutellaria baicalensis Glycoside sodium salt precipitated 4.38 g. Scutellarin sodium salt was added to 60mL water, with Na 2 CO 3 Adjust the pH of the solution to 8.0~9.0 to dissolve all the solution, and then use dilute H 2 SO 4 Adjust the pH to 1.5-2.0, filter, wash the precipitate with pure water until the pH is 6.8-7.5, and dry to obtain 4.13 g of scutellarin with a purity of 99.0%, and the product yield is 86.0%.

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Abstract

The invention provides a scutellarin purifying method, which comprises steps of: first dissolving scutellarin crude product in an alkaline solution to change in a salt; then cooling and crystallizing in an aqueous solution to separate impurities; and acidifying to original molecule state to obtain a purified product with main content more than 99%. In the invention, solubility property of scutellarin sodium salt or sylvite is fully utilized to change a scutellarin refining process into a scutellarin salt separating and purifying process, so as to obtain the high-purity scutellarin product. The method of the invention has few operation steps and a high product yield, and is easy to operate and at low costs; besides water is used as a solvent of crystallization to avoid use of a large amount of organic solvents, so as to enhance production security and facilitate industrialized production.

Description

technical field [0001] The invention belongs to a method for preparing traditional Chinese medicine, and relates to a method for purifying scutellarin based on a salt purification process. Background technique [0002] Scutellarin is also known as baicalein, scutellarin, and scutellarin, and its chemical name is 4'-hydroxybaicalein-7-O-glucuronide. Its plant source is Scutellaria baicalensis (Scutellaria altissima L.), stems and leaves of Scutellaria altissima L., stems and leaves of Scutellaria altissima (S. Barbara D. Don), etc. Clinical research results show that scutellarin has the effects of reducing cerebrovascular resistance, improving cerebral blood circulation, increasing cerebral blood flow and anti-platelet aggregation, and is clinically used for the treatment of paralysis after cerebrovascular disease. [0003] Although scutellarin (scutellarin) has a very clear curative effect on the treatment of ischemic cerebrovascular disease and coronary heart disease, due ...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/06
Inventor 王龙虎梅彦红孙笛陈勇刘雪松
Owner ZHEJIANG UNIV
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