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A method for separating and purifying ginkgolide a and ginkgolide b

A technology of ginkgolide and ginkgo leaf, applied in the direction of organic chemistry and the like, can solve problems such as difficulty in obtaining high purity, and achieve the effects of wide health care range, high product purity and low production cost

Active Publication Date: 2019-04-19
孙焱辉 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purity of multi-stage extraction will continue to improve, but it is difficult to obtain high purity

Method used

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  • A method for separating and purifying ginkgolide a and ginkgolide b
  • A method for separating and purifying ginkgolide a and ginkgolide b

Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0019] 1. Separator operation

[0020] 1. Ginkgo biloba extract powder is weighed and poured into the separator from the hopper.

[0021] 2. Put the concentrated coarse crystal mother liquor (60%) left over from the last purification, the precipitation chamber washing liquid (20%), the single crystal mother liquor (5%) and tap water (15%). The total material-to-liquid ratio is 1:18.

[0022] 3. Heat and start the stirrer, slowly add sodium hydroxide until the pH is about 8.0, the extract powder and lye are in a semi-dissolved state, and GA and GB are activated and dissolved.

[0023] 4. After ten minutes, turn on the separator cooling water, cool to room temperature, slowly put in hydrochloric acid, until PH2.0-2.5, stop stirring, the solution precipitates colloidal impurities

[0024] 5. Decant the liquid and flow to the settling tank.

[0025] 6. Open the slag outlet of the separator, clear out the extract powder residue, and dispose of it.

[0026] 2. Settling tank oper...

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PUM

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Abstract

The invention provides a high-purity and low-cost purification method for separating ginkgolide A and ginkgolide B (GA and GB) from ginkgo extract powder on the basis of the activation characters of the ginkgolide A and ginkgolide B. The method includes the following steps: (1) alkaline-dissolving and heating the ginkgo extract powder and regulating the pH to 7-9, so that the GA and the GB are ring-opened and deformed to form activated GA and GB; (2) adding hydrochloric acid to the alkaline solution containing the activated GA and GB to regulate the pH to 2.0-2.5, and cooling and separating the alkaline solution to obtain a solution and insoluble impurities; (3) adding NaOH to the solution to regulate the pH to about 4-6, so that the activated GA and GB are combined with the impurities to form a GA combined substance and a GB combined substance, thus forming a coarse grain precipitate; and (4) hot-melting the coarse grain with ethanol to decompose the GA and GB, and re-crystallizing the GA and GB to obtain a finish product. The finish product is 22.95% in content of the GA and is 76.15% in content of the GB, total ginkgolic acid being not detected. Due to the high purity, the product can be used as a raw material for high-quality chemical drugs and health-caring products.

Description

Technical field [0001] The invention relates to a method for separating and purifying ginkgolide A (GA) and ginkgolide B (GB) from ginkgo leaf extract powder. Background technique [0002] At present, the separation and purification of ginkgolides from Ginkgo biloba extract powder can be attributed to two methods, extraction and chromatography. Chromatography also includes adsorption, column chromatography, chromatographic simulated moving bed, and preparative chromatography. In addition to the limitation of high production cost of these two methods, the key deficiency is that it is difficult to obtain high-purity GA and GB. In terms of chromatography, since GA and GB are adsorbed by a solid adsorbent and then eluted with a solvent, a part of GA and GB will be denatured, even if the proportion is small. Preparative chromatography can obtain high-purity GA and GB, but it uses nano-scale adsorbents, and the process requirements are very high, which is difficult to meet in la...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/22
CPCC07D493/22
Inventor 孙焱辉孙有成
Owner 孙焱辉
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