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A kind of preparation technology of water-soluble ginkgo leaf extract

A preparation process, the technology of ginkgo biloba, which is applied in the field of preparation of water-soluble ginkgo leaf extract, can solve the problems of large difference in resin adsorption, poor process controllability, limited product application, etc., and achieve stable product quality and simple production process , Good process stability

Active Publication Date: 2011-12-28
ZHEJIANG CONBA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the lactone content of conventional water-soluble Ginkgo biloba extract is about 6-7%, and its cold water (25°C) solubility is about 5%, so it is difficult to further improve the quality, and the product application is limited
[0005] At present, Ginkgo biloba extracts on the market are mainly prepared by resin method, solvent extraction method, etc. After searching, there are more than 90 patent applications related to Ginkgo biloba extracts, such as "CN101524380", a kind of Ginkgo Preparation process, "CN101422493" a preparation method of ginkgo leaf extract and its application, etc. These applications mainly belong to the preparation method of ordinary ginkgo leaf extract, and the patent applications for the preparation process of water-soluble ginkgo leaf extract mainly include 4 Article: The patent application number 02113533.9 introduces a "production process of water-soluble ginkgo leaf extract". The adsorption of esters to resins is quite different, and the water solubility of picrolactone is poor. Therefore, it is difficult to ensure the content of ginkgolide and the water solubility of the extract by using this process.
The patent application number CN200510003243.1 introduces "a production method of water-soluble ginkgo leaf extract". In this process, the GBE crude product is extracted by stirring with water or dilute alcohol, and the filtrate is added to the gelatin aqueous solution to precipitate to prepare water-soluble ginkgo. Leaf extract, due to the poor solubility of ginkgolides in water or dilute alcohol solution, and the precipitation of gelatin, the use of this process to prepare water-soluble extracts will cause a greater loss of active ingredients, especially ginkgolides. The controllability of technology is relatively poor, it is difficult to obtain the stable water-soluble ginkgo leaf extract that meets certain content specifications; the patent application number is 200810060422.2 has introduced " a kind of production technology of water-soluble ginkgo leaf extract ", and this technology uses ginkgo biloba After the common extract is prepared from leaves, it is dissolved in ethanol, heated and extracted for many times, concentrated, then heated and extracted with purified water for many times, the extract is cooled and filtered, and dried. This process requires multiple heating and extraction, which is effective for There is a certain loss of flavonoids, and the simple alcohol extraction and water extraction have a large loss of effective ingredients ginkgolides, especially ginkgolide B and ginkgolide C, which cannot guarantee that ginkgolide B≥0.9% and ginkgolide Ester C ≥ 1.2% injection raw material requirements, while the tannin content is also difficult to meet the requirements; application number is 201010117094.2 patent introduced "a kind of preparation method of water-soluble ginkgo extract", the process adopts ethyl acetate extraction, C2-C8Alkanes are deacidified and prepared in combination with polyamide resin purification. The water-soluble extract is prepared according to this process. The disadvantages are ethyl acetate extraction and The production technology of C2-C8alkane deacidification is relatively high. Ginkgo flavonoids and lactones are prepared separately, and the yield of the finished product is low, and after mixing and drying, The water solubility of the lactone cannot be guaranteed, the process operation is more complicated, the industrialization requirements are higher, and the cost is higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Take 5kg of crushed ginkgo leaves, add 35kg of 60% acetone-water mixed solution, reflux extraction twice, combine the two extracts, concentrate until no acetone; add water to dilute to a density of 1.04g / mL (50°C), let cool, cool Settle (0-10°C) for 8 hours, filter to obtain a clarified filtrate; apply HPD750 macroporous adsorption resin to the filtrate, pre-wash 2BV with purified water, pre-wash 2BV with 10% ethanol, then elute with 65% ethanol for 2BV, and elute with ethanol Liquid, concentrated to get alcohol-free thick paste I; take non-alcoholic thick paste I, add about 8 times the amount of 95% ethanol to dissolve, the alcohol degree is about 81%, let it cool, filter, and concentrate the filtrate to get alcohol-free thick paste II; Thick paste II, add 15 times the amount of purified water, heat and extract for 0.5h, cool to room temperature, refrigerate (0-10°C) for 24h, cool the liquid, filter, concentrate, and dry under reduced pressure to obtain water-soluble gi...

Embodiment 2

[0039] Take 5 kg of crushed Ginkgo biloba leaves, add 35 kg of 60% acetone-water mixed solution, reflux extraction twice, combine the two extracts, concentrate until there is no acetone; add water to dilute to a density of 1.05 g / mL, let cool, and freeze 10°C) for 10 hours, filtered to obtain a clarified filtrate; HPD750 macroporous adsorption resin was applied to the filtrate, pre-washed with purified water for 2BV, 15% ethanol for 2BV, and then eluted with 65% ethanol for 2BV, and the ethanol eluate was taken and concentrated to obtain Alcohol-free thick paste I; take non-alcoholic thick paste I, add about 10 times the amount of 95% ethanol to dissolve, the alcohol content is about 85%, let it cool, filter, concentrate the filtrate, and get non-alcoholic thick paste II; take non-alcoholic thick paste II , adding 15 times the amount of purified water, heating and extracting for 1.0h, cooling to room temperature, refrigerating (0-10°C) for 30h, cooling the liquid, filtering, co...

Embodiment 3

[0042] Take 50 kg of crushed Ginkgo biloba leaves, add 300 kg of 60% acetone-water mixed solution, reflux extraction twice, combine the two extracts, concentrate to no acetone; 10°C) for 8 hours, filtered to obtain a clarified filtrate; the filtrate was applied to HPD750 macroporous adsorption resin, pre-washed with purified water for 2BV, 10% ethanol for 2BV, and then eluted with 65% ethanol for 2BV, and the ethanol eluate was taken and concentrated to obtain Alcohol-free paste I; take alcohol-free paste I, add about 8 amounts of 95% ethanol to dissolve, the alcohol content is about 82%, let it cool, filter, and concentrate the filtrate to obtain alcohol-free paste II; take alcohol-free paste II, Add 10 times the amount of purified water, heat and extract for 0.5h, cool to room temperature, refrigerate (0-10°C) for 24h, cool the solution, filter, concentrate, and spray dry to obtain the water-soluble Ginkgo biloba extract.

[0043] According to the determination of Chinese Ph...

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PUM

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Abstract

The invention relates to a water-soluble ginkgo leaf extract and its preparation technology, The method of the invention comprises: taking common ginkgo biloba as a raw material, mixing with acetone and extracting, concentrating, diluting by adding water, cryoprecipitating, filtering, performing a gradient elution to a filtrate through macroporous adsorption resin, carrying out an alcohol precipitation by ethanol with high purity, water extraction and cryoprecipitating, concentrating, drying to obtain the water-soluble ginkgo leaf extract, wherein the content of total flavonol glycoside is greater than or equal to 27%; the content of lactone content is 9%-12%, wherein the content of Terpene Lactones A is greater than or equal to 2.1%, the content of Terpene Lactones B is greater than or equal to 0.9%, the content of Terpene Lactones C is greater than or equal to 1.2%, and the lactone ratio of GA:GB:GC is close to 7:3:4; the water-solubility is greater than and equal to 10%; the ginkgolic acid is less than and equal to 1ppm, which can be taken as a raw material used for injection. The invention has the advantages of simple production technology, high and stable product quality, high finished product yield, low cost and good economic benefit.

Description

technical field [0001] The invention relates to a preparation process of water-soluble ginkgo leaf extract, which belongs to the technical field of traditional Chinese medicine preparations. Background technique [0002] Ginkgo (ginkgo, Latin name Ginkgobiloba) alias: ginkgo, gongsun tree, duck foot tree, cattail fan, belongs to gymnosperms. Ginkgo biloba has been used as medicine for more than 800 years. As early as the Song Dynasty, Chinese folks used ginkgo biloba to treat asthma and bronchitis. Ginkgo preparations and ginkgo-like health foods are one of the most popular plant products in the world market today. Since the 1960s, scientists from Germany and France took the lead in extracting anti-cardiovascular and cerebrovascular components (gingko flavonoids and ginkgolides) from the leaves of Ginkgo biloba. The Ginkgo preparation represented by Ginkgo biloba has gained a good reputation in the international pharmaceutical market. According to estimates by American ec...

Claims

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Application Information

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IPC IPC(8): A61K36/16A61P9/00A61P7/02A61P9/10A61P25/22A61K127/00
Inventor 叶剑锋姚建标陈玲芳盛卫国吴健马丽萍邱红英
Owner ZHEJIANG CONBA PHARMA
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