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A kind of preparation method of high-content geniposide crystal

A technology of geniposide and high content is applied in the field of preparation of high-content geniposide crystallization, which can solve the problems that the product content cannot meet the requirements of the market, cannot be industrialized, and has small processing capacity, and achieves strong market competitiveness. And the effect of development prospects, short cycle and stable quality

Active Publication Date: 2018-06-08
YUNNAN CHANONG BIOLOGICAL IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preliminary conclusion drawn through comparative research is that the above method is acceptable as a research, but cannot be industrialized
Its main problems are: complex process, excessive material consumption, and low yield. Column chromatography can effectively purify the content of geniposide from 50% to about 95%, but the processing capacity is small and the input cost is too high. The content of the obtained product does not meet the requirements of the market
At present, the domestic price of geniposide crystals is very high, but the supply is very small. Therefore, it is the demand of the market to find and develop a production method that is safe and reliable in the production process, low in production cost, and high in product quality.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Crush the gardenia fruit into coarse powder, add ethanol with a concentration of 70v / v% according to the solid-liquid ratio g / mL of 1:10, extract twice at 60°C, combine the extracts, and diatomaceous earth Adsorption, and then filtered to obtain the filtrate, the filtrate was then concentrated under reduced pressure to obtain geniposide extract;

[0021] (2) ultrasonically extracting the geniposide extract obtained in step (1) with a mixture of ethyl acetate and methanol for 4 times, combining the extracts, and then concentrating under reduced pressure to obtain the crude geniposide; the acetic acid The mixed solution of ethyl acetate and methanol is the mixed solution obtained by mixing analytically pure ethyl acetate and methanol in a volume ratio of 1:2;

[0022] (3) Take 1 kg of the crude geniposide obtained in step (2), and dissolve it in a water bath at 60°C with a methanol solution with a mass concentration of 15% to obtain a saturated solution;

[0023] (4)...

Embodiment 2

[0026] (1) Grind the gardenia fruit into coarse powder, add ethanol with a concentration of 50v / v% according to the solid-liquid ratio g / mL of 1:5, extract once at 50°C, combine the extracts, and diatomaceous earth Adsorption, and then filtered to obtain the filtrate, the filtrate was then concentrated under reduced pressure to obtain geniposide extract;

[0027] (2) Ultrasonic extraction of the geniposide extract obtained in step (1) with a mixture of ethyl acetate and methanol was performed twice, the extracts were combined, and then concentrated under reduced pressure to obtain crude geniposide; the acetic acid The mixed solution of ethyl acetate and methanol is the mixed solution obtained by mixing analytically pure ethyl acetate and methanol in a volume ratio of 1:1;

[0028] (3) Take 1 kg of the crude geniposide obtained in step (2), and dissolve it in a water bath at 60°C with a methanol solution with a mass concentration of 15% to obtain a saturated solution;

[0029]...

Embodiment 3

[0032] (1) Crush the gardenia fruit into a coarse powder, add ethanol with a concentration of 75v / v% according to the solid-liquid ratio g / mL at 1:20, extract three times at 80°C, combine the extracts, and then diatomaceous earth Adsorption, and then filtered to obtain the filtrate, the filtrate was then concentrated under reduced pressure to obtain geniposide extract;

[0033] (2) Ultrasonic extraction of the geniposide extraction extract obtained in step (1) with a mixture of ethyl acetate and methanol for 6 times, combining the extracts, and then concentrating under reduced pressure to obtain the crude geniposide; the acetic acid The mixed solution of ethyl acetate and methanol is the mixed solution obtained by mixing analytically pure ethyl acetate and methanol in a volume ratio of 1:3;

[0034] (3) Take 1 kg of the crude geniposide obtained in step (2), and dissolve it in a water bath at 60°C with a methanol solution with a mass concentration of 15% to obtain a saturated ...

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Abstract

The invention discloses a preparation method of high-content geniposide crystals. The preparation method comprises the steps that cape jasmine fruits are smashed, extracted with ethyl alcohol, adsorbed with kieselguhr and then concentrated to obtain geniposide extracting extractum; extracting is performed with a mixed solution of ethyl acetate and methyl alcohol to obtain crude geniposide; the crude geniposide is dissolved with a methyl alcohol solution to obtain a saturated solution, cooling is performed after immediate filtration is performed, analytically pure ethyl acetate is added for first-time stirring crystallizing, solution adding is stopped, standing is performed for several hours, the analytically pure ethyl acetate is added for second-time stirring crystallizing until acicular crystals stop growing, a crystallizing system is obtained, and after filtering and reduced-pressure drying are performed, the snowy white acicular geniposide crystals are obtained. According to the crystals obtained through the method, it is detected that the geniposide purity can be more than 98.8 percent, and no toxic substance residue exists. The preparation method is mild in condition, low in cost and high in speed, has the advantages of being safe in production process, easy and convenient to operate, low in cost, short in cycle, high in product quality and stable in quality, and is suitable for industrialized production.

Description

technical field [0001] The invention relates to a method for preparing high-content geniposide crystals, and belongs to the technical field of plant extraction and purification. Background technique [0002] Gardenia, also known as yellow gardenia, mountain gardenia, and white toad, is the fruit of the Rubiaceae plant gardenia. Gardenia contains more than 40 kinds of physiologically active substances, among which the active ingredients of Gardenia, a traditional Chinese medicine recognized at home and abroad, are iridoids. The iridoids contained in gardenia include geniposide, geniposide, hydroxygeniposide, geniposide, etc., among which the highest active ingredient is geniposide or geniposide. Geniposide is hydrolyzed into geniposide (geniposide) by β-glucosidase, that is, geniposide must be metabolized into geniposide in the intestinal tract before it can exert its curative effect. Convenience, relief of type II diabetes, anti-inflammatory, anti-thrombosis, anti-tumor, a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/04C07H1/08
Inventor 李定忠
Owner YUNNAN CHANONG BIOLOGICAL IND
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