Preparation technology of low-acidity and high-purity terpene lactone extract in gingko root and bark

A preparation process and technology for terpene lactones are applied in the field of preparation of low-acid and high-purity terpene lactone extracts, which can solve the problems of large market demand, certain hidden dangers in safety, and unsuitability for mass preparation, etc. The effect of high product quality, stable product quality and low production cost

Active Publication Date: 2014-03-05
ZHEJIANG CONBA PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some studies also focus on the separation of GA and GC monomers, such as patent 201010294667.9 "A Production Process for Extracting Ginkgolides A and C from Ginkgo Root Bark" and 201110067186.9 "Isolation and Purification of Ginkgolides from Ginkgo Root Bark Method C", the process of monomer preparation and separation is relatively complicated, and at the same time other terpene lactone components are

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044]Ginkgo root bark, remove impurities, crush to coarse powder (through 24 mesh sieve), take 100 kg of ginkgo root bark coarse powder, add 1000 kg of ethanol with a mass fraction of 60%, heat and reflux for extraction twice, combine the two extracts, and decompress Concentrate until alcohol-free (ethanol content is less than 5%) to obtain a concentrated solution; add water to dilute to a density of 1.0g / mL at 50°C, absorb on a 100-mesh polyamide adsorption resin on the diluted solution, and elute with purified water of 3 times the column volume , collect the adsorption residue and water eluent, concentrate under reduced pressure to a density of 1.25g / mL (50°C) to obtain a thick paste; add a certain amount of ethanol to a solution concentration of 20%, and heat it in a water bath at 60°C to dissolve completely. Filtrate, put the filtrate in the refrigerator quickly for 8 hours, recrystallize, and the refrigerator temperature is 0-4°C; after recrystallization, the mother liquo...

Embodiment 2

[0046] Take 100kg of ginkgo root bark powder, add 1200kg of 80% ethanol, heat and reflux for extraction 3 times, combine the two extracts, concentrate under reduced pressure to no alcohol, dilute with water to a density of 1.05g / mL at 50°C, and add 200 The polyamide adsorption resin is adsorbed, and eluted with 4 times the column volume of purified water, the adsorption residue and water eluate are collected, concentrated under reduced pressure to a density of 1.42g / mL (50°C), and a certain amount of ethanol is added to the solution concentration to 40%, heated in a water bath at 60°C to dissolve completely, filtered, and the filtrate was quickly refrigerated for 12 hours for recrystallization. After recrystallization, the mother liquor was recrystallized repeatedly 3 times, and all crystals were combined to obtain crude crystals. The crude crystals were separated by high-performance liquid chromatography, and the samples were injected repeatedly. The five lactone fractions be...

Embodiment 3

[0048] Take 500kg of ginkgo root bark powder, add 7500kg of 70% ethanol, heat and reflux for extraction 3 times, combine the two extracts, concentrate under reduced pressure to no alcohol, dilute with water to a density of 1.10g / mL at 50°C, and add 300 The polyamide adsorption resin is adsorbed, and eluted with 4 times the column volume of purified water, the adsorption residue and water eluate are collected, concentrated under reduced pressure to a density of 1.31g / mL (50°C), and a certain amount of ethanol is added to the solution concentration 30%, heated in a water bath at 60°C to dissolve it completely, filtered, and the filtrate was quickly refrigerated for 10 hours and recrystallized. After recrystallization, the mother liquor was recrystallized repeatedly 3 times, and all crystals were combined to obtain crude crystals. The crude crystals were separated by high-performance liquid chromatography, and the samples were injected repeatedly. The five lactone fractions betwe...

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Abstract

The invention discloses a preparation technology of a low-acidity and high-purity terpene lactone extract in gingko root and bark. The technology comprises the following steps: by taking gingko root and bark as raw materials, crushing into coarse powder; adding high-concentration ethanol to extract, concentrating, adding water to dilute, adsorbing by polyamide adsorption resin and eluting; concentrating an eluate, recrystallizing by ethanol, and separating the obtained coarse crystal by high-performance liquid chromatography, so as to prepare the terpene lactone extract, wherein the total lactone content is greater than or equal to 95%, and the total ginkgo acid content is smaller than or equal to 1ppm. By adopting the method disclosed by the invention, the defects of the existing production technology are overcome, and the method has the characteristics of being stable and controllable in production technology, simple and convenient to operate, high and stable in product quality, high in product yield, low in production cost and the like; the gingko root and bark can be changed into precious resources, so as to fully exert the economical value.

Description

technical field [0001] The invention relates to a preparation process of a low-acid high-purity terpene lactone extract from ginkgo root bark, and belongs to the technical field of traditional Chinese medicine preparations. Background technique [0002] Ginkgolides are a kind of important active compounds unique to Ginkgo biloba leaves and Ginkgo root bark. They are composed of sesquiterpene lactones and diterpene lactones. , Ginkgolide J and Bilobalide. Ginkgolic acid (GA) is a toxic and side effect component in Ginkgo biloba extract. It has sensitization, cytotoxicity and immunotoxicity, and has potential hazards to human health. It mainly exists in Ginkgo biloba, Ginkgo fruit and Ginkgo root bark; Germany began to strictly limit the GA level in ginkgo biloba preparations to below 5ppm in 1997. The European Pharmacopoeia continued to use the GA limit requirement of 5ppm in the GBE standard, and the 2010 edition of the Chinese Pharmacopoeia also limited the GA content in G...

Claims

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Application Information

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IPC IPC(8): A61K36/16A61K127/00
Inventor 姚建标王如伟叶剑锋方玲吴旭明金辉辉胡林水
Owner ZHEJIANG CONBA PHARMA
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