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Ginkgoic acid preparation method using macroporous adsorption resin

A ginkgolic acid and pore adsorption technology, which is applied in the separation/purification of carboxylic acid compounds, antiviral agents, anti-infective drugs, etc., can solve the problems of large solvent consumption, poor solvent permeability, and high preparation cost, and achieve improved purity and quality, shorten preparation time, and reduce preparation cost

Inactive Publication Date: 2009-09-16
FUZHOU UNIV
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Problems solved by technology

But, the technology that this adopts lipophilic organic solvent extraction, silica gel column chromatography purification or HPLC preparative chromatogram to prepare ginkgolic acid by methods such as multiple separations has the disadvantages that the permeability of lipophilic solvent is not strong, the consumption of solvent and silica gel is large, and the solvent Disadvantages of high toxicity, high preparation cost, large investment in equipment, and difficult implementation of industrialized safe production
[0011] There are also scholars in China who improve the deficiencies of the above-mentioned process, and use 80% industrial ethanol to extract ginkgolic acid instead, then use macroporous adsorption resin to refine, and ethanol gradients of different concentrations elute ginkgolic acid [Ni Xuewen et al. Research on acid, Chinese herbal medicine, 2003, 34(3): 231-233; Ni Xuewen et al., Extraction method of ginkgolic acid from Ginkgo testa and its antitumor activity in vitro, Jiangsu Agricultural Science, 2006(5): 151-153] , but because ginkgolic acid is a fat-soluble compound, it is difficult to dissolve in polar solvents such as water, methanol, ethanol, and the technology of using this non-alkaline ethanol aqueous solution to extract and elute ginkgolic acid still has solvent permeability is not strong, solvent Disadvantages of large consumption, high solvent toxicity, high preparation cost, low yield and purity of ginkgolic acid

Method used

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  • Ginkgoic acid preparation method using macroporous adsorption resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Ginkgo biloba extract material solution with a ginkgolic acid concentration of 3.2mg / ml, use HZ802 macroporous adsorption resin to absorb ginkgolic acid to saturation, first wash off the residual material solution that is not adsorbed by the resin with 2 times the volume of the resin, and then use 3 times the resin volume The 30% methanol aqueous solution of pH7.0 of volume washes away the impurity that is weaker than ginkgolic acid with HZ802 resin adsorption force, finally elutes the ginkgolic acid component with 45% methanol aqueous solution of pH11.2 of 3.5 times of resin volume, and eluent adjusts After the pH value reaches 6.5-7.0, the solvent is recovered under reduced pressure, concentrated in vacuo, separated from the upper layer oil, and dried to obtain the finished product of ginkgolic acid. After determination, the recovery rate of ginkgolic acid was 95.2%, and the purity of ginkgolic acid was 86.7%.

Embodiment 2

[0038] Ginkgo biloba extract extract containing 400ppm ginkgolic acid, under the condition of 65 ℃, with 6 times the volume of 95% ethanol aqueous solution with pH8. .1, after ethanol concentration 48% and ginkgolic acid concentration 0.16mg / ml, use AB-8 macroporous adsorption resin to adsorb ginkgolic acid to saturation, first wash off the residual material liquid that is not adsorbed by resin with water of 3.5 times of resin volume, and then Use the 35% ethanol aqueous solution of pH7.0 of 4.2 times of resin volume to wash away and the impurity weaker than ginkgolic acid with AB-8 resin adsorption force, finally use the 63% ethanol aqueous solution of pH9.0 of 5.1 times of resin volume to elute the ginkgolic acid group After the pH value of the eluent was adjusted to 7.0, the solvent was recovered under reduced pressure, concentrated in vacuo, the upper layer oil was separated, and dried into a finished product of ginkgolic acid. After determination, the recovery rate of gin...

Embodiment 3

[0040] Ginkgo biloba extract powder containing 2000ppm ginkgolic acid, under the condition of 60 ℃, with 3 times the volume of 60% methanol aqueous solution with pH9. 9. After the concentration of methanol is 54% and the concentration of ginkgolic acid is 0.48mg / ml, use HZ801 macroporous adsorption resin to absorb ginkgolic acid to saturation. The 40% methanol aqueous solution of pH 7.0 of the resin volume washes away the impurity with HZ801 resin adsorption force weaker than ginkgolic acid, finally elutes the ginkgolic acid component with 56% methanol aqueous solution of pH 10.1 of 4.8 times the resin volume, and the eluent After adjusting the pH value to 3.2, recover the solvent under reduced pressure, concentrate in vacuo, separate the oil in the upper layer, and dry it to obtain the finished product of ginkgolic acid. After determination, the recovery rate of ginkgolic acid was 96.1%, and the purity of ginkgolic acid was 85.2%.

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Abstract

The invention provides a ginkgoic acid preparation method using macroporous adsorption resin, comprising the following steps: absorbing ginkgoic acid from the feed liquid containing ginkgoic acid until being saturated using the macroporous adsorption resin; using water to wash out the residual feed liquid which is not absorbed by the resin; washing the impurities with lower resin absorption compared with the ginkgoic acid using the non-alkaline hydrophilic organic solvent aqueous solution; eluting ginkgoic acid constituents using the non-acidity hydrophilic organic solvent aqueous solution; adjusting the p H value of the eluent; decompression recovering the solvent and vacuum concentrating and drying the eluent to produce the finished products of the ginkgoic acid. The preparation method has features of novel design, simple and easily executed technology, best quality, low production cost, and can be used in further separation and purification of the feed liquid containing ginkgoic acid from separate sources with larger generalization.

Description

technical field [0001] The invention relates to a method for separating and purifying natural products, more specifically to a method for preparing natural product ginkgolic acid by using a macroporous adsorption resin. Background technique [0002] Ginkgo biloba is a rare and precious tree species unique to China. It is known as the "living fossil of the plant kingdom". It is listed as a national second-class protected plant and is included in the first batch of Chinese herbal medicines with the same origin of medicine and food. China's ginkgo resources account for the world's total 70% of. [0003] Both ginkgo fruit and ginkgo leaves have high medicinal value and edible value. Modern pharmacological research shows that its active ingredients mainly include flavonoids, lactones, ginkgolic acid and polyprenol. Vascular disease, senile peripheral circulation disorder, senile dementia have good curative effect, and ginkgolic acid and polyprenol have obvious anti-tumor, anti-o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C65/05C07C51/47A61P35/00A61P39/06A61P31/00A61P31/12A61P29/00
Inventor 陈剑锋
Owner FUZHOU UNIV
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