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Preparation method of baohuoside I

A technology of baohuoside and icariin, which is applied in the field of preparation of baohuoside I, can solve the problems of low conversion rate, complicated operation, difficult separation and purification, and achieve improved reaction efficiency, high enzymatic hydrolysis reaction efficiency, and dissolution fast speed effect

Inactive Publication Date: 2012-01-11
贾晓斌
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The conversion ability of this method is not strong, the operation is complicated, time-consuming, and the conversion rate is low, separation and purification are difficult, which is not conducive to industrial production

Method used

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  • Preparation method of baohuoside I
  • Preparation method of baohuoside I

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 2 g of icariin (purity 95.7%) and dissolve it in 500 mL of 50% ethanol, and dissolve 0.5 g of β-glucosidase in 330 mL of water, slowly add the dilute ethanol solution of icariin into the enzyme aqueous solution, The concentration of ethanol was diluted to 30%, stirred at 37°C for 6 hours, the reaction solution was evaporated in vacuo to remove the solvent, and the conversion rate of icariin was detected by high performance liquid phase method. As a result, 98.5% of icariin was converted into Huoside I.

[0024] Take 2 g of icariin (purity 95.7%) and 0.5 g of β-glucosidase, disperse them in 830 mL of water, stir at 37 ° C for 6 hours, evaporate the reaction solution in vacuum, remove the solvent, and detect the epimedium by HPLC The conversion rate of glycosides showed that 36.3% of icariin was converted into baohuoside I.

[0025] Take 2 g of icariin (purity 95.7%) and 0.5 g of β-glucosidase, disperse them in 830 mL of 30% ethanol, stir at 37° C. for 6 hours, evap...

Embodiment 2

[0027] Dissolve 2 g of icariin (purity 95.7%) in 500 mL of 50% dilute ethanol, and dissolve 0.5 g of β-glucosidase in 330 mL of water, slowly add the dilute ethanol solution of icariin into the enzyme aqueous solution , dilute the ethanol concentration to 30%, and stir at 37° C. for 6 hours. After the reaction, add an equal amount of ethanol to precipitate β-glucosidase, filter the filtrate, and evaporate the solvent to obtain 1.52 g of Baohuoside I crude product. Repeated recrystallization with absolute ethanol 3 times to obtain 1.08 g of baohuoside I with a purity of 99.5%.

[0028] Take 2 g of icariin (purity 95.7%) and 0.5 g of β-glucosidase, disperse them in 830 mL of water, stir at 37°C for 6 hours, add an equal amount of ethanol to precipitate β-glucosidase after the reaction, and filter to get the filtrate , Evaporate the solvent to get 1.72g of the crude product of Dibaohuoside I. Repeated recrystallization with absolute ethanol 3 times to obtain 0.31 g of baohuoside...

Embodiment 3

[0033] Take 2 g of icariin (purity 65.7%) and dissolve it in 500 mL of 50% dilute ethanol, and dissolve 1 g of cellulase in 330 mL of water. Slowly add the dilute ethanol solution of icariin into the enzyme aqueous solution to make ethanol Dilute the concentration to 30%, and stir at 40°C for 12 hours. After the reaction, add an equal amount of ethanol to precipitate the cellulase, filter the filtrate, and evaporate the solvent to obtain 1.55 g of the crude product of Baohuoside I, which is absorbed by D101 macroporous resin , eluted with water, 30% ethanol, and 60% ethanol respectively, collected the 60% ethanol part, vacuum rotary evaporation, removed the solvent, repeated recrystallization 2 times from absolute ethanol, and obtained 0.55 g of baohuoside I with a purity of 99.2%.

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Abstract

The invention provides a preparation method of baohuoside I, which has a high efficiency and a high conversion rate. The method is characterized in that baohuoside I is obtained by treating a certain concentration of ethanol as a reaction medium, and carrying out enzyme hydrolysis on icariin. The method which adopts a low concentration of an ethanol solution as the reaction medium has the advantages of increase of the specific surface area of a contact reaction of icariin with an enzyme, shortening of the reaction time, improvement of the conversion efficiency and the conversion rate, simple and feasible technology, good purposiveness, no pollution, and realization of industrial production, and overcomes disadvantages of complex operation, much time consumption, low conversion rate, bad purposiveness, difficult separation and purification, and the like existing in the prior art.

Description

technical field [0001] The invention relates to a preparation method of baohuoside I, which belongs to the technical field of medicine. Background technique [0002] Epimedium has a long history of medicinal use and has definite curative effects. It is a commonly used traditional Chinese medicine in clinical practice. Its traditional functions are to invigorate kidney yang, strengthen muscles and bones, and dispel wind-dampness. For impotence and nocturnal emission, flaccidity of muscles and bones, rheumatic arthralgia, numbness and contracture. Modern pharmacological experiments have shown that Epimedium can enhance cardiovascular and cerebrovascular blood flow, promote hematopoietic function, regulate bone metabolism, improve immune function, and also has various effects such as anti-aging, anti-tumor and anti-AIDS. Mass loose, climacteric syndrome, high blood pressure, coronary heart disease, polio, chronic bronchitis and other diseases. Because of its rich medicinal p...

Claims

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Application Information

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IPC IPC(8): C12P19/60C07H17/07C07H1/06
Inventor 贾晓斌孙娥张振海朱粉霞陈玲玲
Owner 贾晓斌
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