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Method for preparing shikimic acid from folium ginkgo extraction waste liquor

A technology of Ginkgo biloba and shikimic acid, applied in the separation/purification of carboxylic acid compounds, organic chemistry and other directions, can solve problems such as low yield of shikimic acid, poor product quality, and complicated operation, and achieves satisfying purity requirements and process design. Reasonable and simple preparation process

Active Publication Date: 2019-04-09
GUILIN NATURAL INGREDIENTS CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extraction of shikimic acid from ginkgo waste liquid is usually carried out by solvent extraction, silica gel column chromatography and anion exchange resin adsorption. However, the above methods are cumbersome to operate, and the yield of shikimic acid obtained from the extraction is low, the content is low, and the quality of the product is not good.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add cellulase to 100g of ginkgo biloba extract waste liquid, the amount of cellulase is 0.1g, enzymolyze at 45°C for 3 hours to obtain enzymolysis solution, pass the enzymolysis solution through an organic membrane, first pass through an organic membrane with a molecular weight of 8000 Membrane, the membrane inlet pressure is 0.5MPa, and the organic membrane of 800 molecular weight is passed through, the membrane inlet pressure is 2.0MPa, and the decolorization membrane solution is obtained, and the membrane fluid directly enters strongly basic anion resin D290 (Tianjin Nankai Resin Factory), after entering Use 4 times the column volume of 0.5mol / L hydrochloric acid solution to elute and separate, and collect from the time when the pH of the effluent is less than 7. The effluent was concentrated under reduced pressure to a solid content of 55% brix in the concentrated solution, adjusted to pH = 1.0 with 4% volume fraction hydrochloric acid solution, and crystallized at 4...

Embodiment 2

[0033] Add pectinase and papain to 100g of ginkgo leaf extraction waste liquid, the total amount of pectinase and papain is 0.2g, enzymolyze at 50°C for 1 hour to obtain enzymolysis solution; pass the enzymolysis solution through organic membrane , first pass through an organic membrane with a molecular weight of 8000, and the membrane inlet pressure is 0.48MPa, and then pass through an organic membrane with a molecular weight of 800, and the membrane inlet pressure is 1.9MPa, to obtain a decolorized membrane solution; the membrane fluid directly enters strongly alkaline anion resin D296 (Tianjin Nankai Resin factory), after entering, use 3 times column volume 0.8mol / L formic acid solution to elute and separate, and start to collect from the effluent pH less than 7. The resulting effluent was concentrated under reduced pressure until the solid content in the concentrate was 58% brix, adjusted to PH=1.5 with 4% volume fraction of formic acid, and crystallized at 8°C for 10 hours...

Embodiment 3

[0035] Add pectinase, cellulase, papain total three kinds of enzymes in 100g of ginkgo leaf extraction waste liquid, these three kinds of enzymes total dosages are 0.8g, enzymolysis 2 hours at 60 ℃ of temperature, obtain enzymolysis solution, will The enzymatic hydrolysis solution passes through the organic membrane, first passes through the organic membrane with a molecular weight of 8000, and the membrane inlet pressure is 0.45MPa, and then passes through an organic membrane with a molecular weight of 800, and the membrane inlet pressure is 1.8MPa to obtain a decolorization membrane fluid, which is directly fed into a strong alkaline Anion resin D201 (Tianjin Nankai Resin Factory) was eluted and separated with 6 times column volume of 0.1mol / L acetic acid solution after entering, and collected from the effluent pH less than 7. The resulting effluent was concentrated under reduced pressure until the solid content in the concentrated solution was 60% brix, adjusted to pH = 1.2 ...

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Abstract

The invention relates to the field of extraction and purification of plant effective components, in particular to a method for preparing shikimic acid from folium ginkgo extraction waste liquor. The method comprises the following steps: carrying out enzymolysis on the folium ginkgo extraction waste liquor; and collecting an enzymatic hydrolysate, filtering by an organic membrane, carrying out adsorption elution by an anion exchange resin column, concentrating, crystallizing and drying. The method is simple to operate, economical and practical and proper to popularize, and does not need an organic solvent. Moreover, the obtained shikimic acid is high in purity and good in appearance condition, and the mass content is greater than 99%.

Description

technical field [0001] The invention relates to the field of extraction and purification of plant active ingredients, in particular, it provides a method for preparing shikimic acid from ginkgo leaf extraction waste liquid. Background technique [0002] The molecular formula of shikimic acid is C7H10O5, and its scientific name is 3,4,5-trihydroxy-1-cyclohexene-1-carboxylic acid, which is a hydroxy acid. Shikimic acid is an intermediate in the synthesis of biological and metabolic compounds, and it is also a raw material for the synthesis of many alkaloids, aromatic amino acids and indole derivatives, and chiral drugs (such as antiviral drugs). [0003] The 2015 edition of "Chinese Pharmacopoeia" stipulates that Ginkgo biloba extract is obtained by subjecting Ginkgo biloba extract to macroporous adsorption resin column chromatography, washing and eluting with water and ethanol aqueous solution in sequence, collecting the eluate, concentrating and drying. In this process, the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/42C07C51/43C07C51/47C07C62/32
CPCC07C51/42C07C51/43C07C51/47C07C2601/16C07C62/32
Inventor 赵军杨文国谢永富宋云飞
Owner GUILIN NATURAL INGREDIENTS CORP
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