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Preparation method for high-purity jasminoidin

A high-purity technology of geniposide, which is applied in the field of preparation of high-purity geniposide, can solve problems such as low yield, complex process, and excessive material consumption, and achieve high product yield and purity, simple operation method, The effect of short production cycles

Inactive Publication Date: 2011-10-12
GUANGXI UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Lead salt precipitation method, silica gel adsorption method, supercritical CO- 2 The fluid method is acceptable as a research, but it cannot be used for industrial production
The main problems are: complex process, excessive material consumption, low yield, and a large amount of toxic and harmful reagents, such as ether, chloroform, methanol, acetone, lead salt, etc.
Utilize the conventional extraction method to enrich geniposide, and then use macroporous adsorption resin to refine and prepare high-purity geniposide. Although compared with the traditional macroporous adsorption resin method, the output per unit time can be obviously improved, but it is still not reached. relatively satisfactory effect

Method used

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  • Preparation method for high-purity jasminoidin

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Effect test

Embodiment 1

[0019] Weigh 100g (dry weight) of gardenia coarse powder, ultrasonically extract 3 times at room temperature, add 500g distilled water for extraction for 1 hour each time, combine three extracts and concentrate under reduced pressure, and concentrate to obtain gardenia with a solid weight content of 30%. Extract the concentrate. At room temperature, adjust the pH value of the gardenia extract concentrate to 9 with sodium carbonate, stir the gardenia extract concentrate at a speed of 400 rpm, and then use the same volume of the extracted gardenia extract concentrate each time Under the condition of n-butanol at a rotating speed of 400 r / min, stir and extract the concentrated solution of Gardenia jasminoides extract, extract twice for 30 minutes each time, and combine the n-butanol extracts. The extract is decolorized with granular activated carbon. After decolorization, the extract is clear and transparent, and the decolorized extract is concentrated under reduced pressure to a...

Embodiment 2~ Embodiment 16

[0021] Weigh 100g (dry weight) of gardenia coarse powder, ultrasonically extract 3 times at room temperature, add 500g distilled water for extraction for 1 hour each time, combine three extracts and concentrate under reduced pressure, and concentrate to obtain a solid content of 30% to 60% by weight (Condition 1) Gardenia extract concentrate. At room temperature, use sodium carbonate to adjust the pH value of the gardenia extract concentrate to 9~11 (condition 2), stir the gardenia extract concentrate at a speed of 400~600 rpm (condition 3), and then use it each time With the same volume of n-butanol or isoamyl alcohol (condition 4) as the extracted gardenia extract concentrate, stir and extract the gardenia extract concentrate at a speed of 400-600 rpm, and extract for 20-60 minutes each time (Condition 5), extract 2 to 6 times (Condition 6), and combine n-butanol or isoamyl alcohol extracts. The extract is decolorized with granular activated carbon. After decolorization, th...

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Abstract

The invention relates to a preparation method for high-purity jasminoidin, particularly a preparation method for high-purity jasminoidin based on liquid-liquid partitioning extraction, which comprises the following steps: pulverizing gardenia, soaking in water, carrying out ultrasonic-assisted extraction, filtering, combining the extraction liquids, and concentrating while depressurizing to obtain a gardenia extraction concentrate; regulating the pH value of the gardenia extraction concentrate to alkaline, and extracting while stirring at high speed by using a low-carbon alcohol as a solvent, thus obtaining an extraction liquid rich in jasminoidin; decolorizing the obtained extraction liquid, and concentrating the decolorized extraction liquid while depressurizing to obtain a decolorized concentrate; pouring the decolorized concentrate into an organic acid ester while stirring so as to crystallize and precipitate jasminoidin; and separating out crystallized jasminoidin precipitate, washing with the organic acid ester, and repeatedly washing the precipitate to obtain the high-purity jasminoidin. The preparation method provided by the invention completely discards chromatography, has the advantages of simple operation process, short production period, high efficiency and high yield and purity of the product, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing high-purity geniposide, in particular to a method for preparing high-purity geniposide based on liquid-liquid distribution and extraction. Background technique [0002] Gardenia is an evergreen shrub of the Rubiaceae Gardenia genus, also known as Mudan, Shanzhi, etc., widely distributed in southern China. Gardenia fruit is dark red or yellow-red, and is commonly used as traditional Chinese medicine in my country. "Compendium of Materia Medica" has detailed records: gardenia fruit has the functions of clearing heat and purging fire, promoting gallbladder and protecting liver, lowering blood pressure, anti-inflammatory and bactericidal, and anti-thrombosis. There are many chemical components in gardenia, among which geniposide and gardenia yellow pigment are the substances with higher content. Geniposide is an active ingredient in Gardenia jasminoides, an effective monomer for the production of gardenia b...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
Inventor 韦万兴朱建文卓家雄周敏朱梅
Owner GUANGXI UNIV
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