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Method for removing ginkgolic acid from ginkgo biloba extract

A technology for ginkgo biloba leaves and extracts, applied in the field of traditional Chinese medicine preparation, can solve the problems of inability to guarantee uniform and stable product quality, unfriendly operators and the environment, organic solvent residues and the like, and achieve uniform and stable product quality, low production cost, and increased content Effect

Active Publication Date: 2012-08-01
JIANGSU SHENLONG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method is prone to emulsification and leads to incomplete extraction, which cannot ensure uniform and stable product quality, and involves organic solvent residues, and is not friendly to operators and the environment.
The patent application (200710049086.7) adopts the superimposed removal method of polyamide and ion exchange resin, which can reduce the content of ginkgolic acid to below 5ppm, but the operation is cumbersome

Method used

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  • Method for removing ginkgolic acid from ginkgo biloba extract
  • Method for removing ginkgolic acid from ginkgo biloba extract

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Dried Ginkgo biloba extract 1kg, crushed to pass through a 100-mesh sieve, stirred and extracted 3 times with hot water at 60°C, each time the amount of water was 3 times the dry weight of Ginkgo biloba extract, extracted for 2 hours each time, filtered, and combined for 3 The second filtrate was used to adjust the relative density to 1.05 with water to obtain an extract. Add 2ml of extract per gram of resin, pass through LSA-10 macroporous adsorption resin exchange column, the ratio of column diameter to height is 1:8, first wash with 3 times the volume of purified water, and then use 16 times the volume of the column, mass The ethanol solution with a percentage concentration of 65% is eluted at a speed of 20ml / min, the eluate is collected, and the ethanol is recovered under reduced pressure to obtain a concentrated solution. The concentrated solution is vacuum-dried below 60°C to obtain about 930g dry extract powder. The yield is 93%. According to the "Chinese Pharma...

Embodiment 2

[0031] Dried Ginkgo biloba extract 2kg, crushed to pass through a 100-mesh sieve, ultrasonically extracted 5 times with 50°C hot water, each time the amount of water was twice the weight of Ginkgo biloba extract, extracted for 1.5 hours each time, filtered, and combined 5 times filtrate, and then adjust the relative density of the filtrate to 110 with water to obtain an extract. Add 2.5 ml of extract per gram of resin, and pass through LSA-21 macroporous adsorption resin exchange column with a diameter-to-height ratio of 1:9. First wash with 4 times the volume of purified water, then elute with 18 times the volume of the column and ethanol solution with a concentration of 70% by mass at a rate of 25ml / min, collect the eluate, recover ethanol under reduced pressure, and obtain a concentrated solution, which is sprayed Dried to obtain about 1910g of dry extract powder, the yield was 95.5%. According to the "Chinese Pharmacopoeia" 2010 edition Ginkgo biloba extract content deter...

Embodiment 3

[0033] Dried Ginkgo biloba extract 2.5kg, crushed to pass through a 100 mesh sieve, stirred and extracted with 40°C hot water for 4 times, each time the amount of water was 2.5 times the weight of Ginkgo biloba extract, extracted for 2 hours each time, filtered, combined 4 The second filtrate was used to adjust the relative density to 1.08 with water to obtain an extract. The ratio of adding 3ml extract per gram of resin is passed through LSA-5B macroporous adsorption resin exchange column, and the diameter-height ratio of the column is 1:10. First wash with 2 times the volume of purified water, then use 17 times the column volume mass percentage concentration of 80% ethanol solution to elute at a speed of 30ml / min, collect the eluate, and recover the ethanol under reduced pressure to obtain a concentrated solution. After drying in vacuum below ℃, about 2.14kg of dry extract powder was obtained, and the yield was 85.6%. According to the "Chinese Pharmacopoeia" 2010 edition Gi...

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Abstract

The invention discloses a method for removing ginkgolic acid from a ginkgo biloba extract. The method comprises the following steps of: extracting, performing column chromatography, and drying, wherein the column chromatography process comprises the following steps of: regulating the relative density of a filtrate obtained by extracting and filtering by using water to be 1.05 to 110 to obtain an extracting solution, allowing the extracting solution to pass through a macroporous adsorption resin exchange column in a ratio of adding 1.5 to 3 milliliters of extracting solution into each gram of resin, washing by using the water, eluting by using 60 to 80 mass percent ethanol solution, and collecting 60 to 80 mass percent ethanol eluent, wherein the macroporous adsorption resin is an LSA series macroporous adsorption resin. According to the ginkgo biloba extract obtained by the method, the content of total flavonol glycosides is more than 35 percent, the content of total terpene lactones is more than 12 percent, and the content of total ginkgolic acid is less than 1 ppm.

Description

technical field [0001] The invention belongs to the technical field of traditional Chinese medicine preparation, and in particular relates to a process for removing ginkgolic acid from ginkgo leaf extract by macroporous adsorption resin column chromatography. Background technique [0002] Ginkgo biloba is a unique species in my country, and its resources account for 70% of the world's total. It has a medicinal history of more than 600 years in my country, and it is also one of the most studied natural plants in western countries. Modern pharmacological studies have shown that the active ingredients in Ginkgo biloba extract are mainly ginkgo flavonoids and terpene lactones. It can be used for the treatment of blood stasis type chest pain and dizziness caused by mild cerebral arteriosclerosis as well as coronary heart disease, angina pectoris, myocardial infarction and other diseases. However, the currently commercially available Ginkgo biloba extracts contain a large amount ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/16B01D15/08A61P9/10A61P25/00A61K127/00
Inventor 秦勇金春胡传良段绪红徐成周自桂苏晋
Owner JIANGSU SHENLONG PHARMA
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