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A kind of preparation method of baohuoside I

A technology of baohuoside and epimedium extract, which is applied in the field of preparation of baohuoside Ⅰ, can solve the problems of unsuitability for industrial production, low yield, waste of medicinal materials, etc., and achieve easy industrial production, good selectivity, and impurity little effect

Active Publication Date: 2021-01-26
BEIJING SHENOGEN BIOMEDICAL
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Problems solved by technology

[0008] In the method provided by the Chinese patent with application number 200780034447.9, baohuoside I was purified using chloroform which is more toxic; in the method provided by the Chinese patent with application number 201110186207.9, Tween was used to The solubility of baohuoside increases the preparation cost; the method described in the Chinese patent application number 201210345102.8 is to directly extract baohuoside I from Epimedium, because the content of baohuoside I in Epimedium is extremely low , generally no more than 0.2%, therefore, the direct extraction method will lead to a lower yield, a serious waste of medicinal materials, and is not suitable for industrial production

Method used

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  • A kind of preparation method of baohuoside I
  • A kind of preparation method of baohuoside I
  • A kind of preparation method of baohuoside I

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Embodiment 1

[0039] 1. Preparation of baohuoside Ⅰ by enzymatic hydrolysis

[0040] Take 10g of Epimedium extract containing 90% icariin, dissolve it in 140mL pH=5.9, 1 / 15M potassium dihydrogen phosphate-disodium hydrogen phosphate buffer solution, add 60mL 95% ethanol under stirring condition, add 100mL fruit Glue enzyme solution, after mixing evenly, start timing when the temperature is constant at 52-55°C, stop the reaction after 48 hours of reaction, and cool the reaction solution to 30°C.

[0041] 2. Purification of Baohuoside I

[0042] After the enzymolysis reaction, the reaction solution was centrifuged to collect the filter cake, which weighed 7.55 g after drying, added 176 g of acetone after crushing, filtered after stirring for 1 hour, added 129 g of purified water to the acetone solution, and heated to reflux until the solution was clear. Then the solution was slowly cooled to 14° C. and kept warm for 2 hours, filtered, and the filter cake was collected and dried to obtain...

Embodiment 2

[0044] 1. Preparation of baohuoside Ⅰ by enzymatic hydrolysis

[0045] Take 3.75kg of Epimedium extract containing 94% icariin, dissolve it in 52L pH=5.9, 1 / 15M potassium dihydrogen phosphate-disodium hydrogen phosphate buffer solution, add 24L 95% ethanol under stirring condition, 75L Pectinase solution, after mixing evenly, start timing when the temperature is constant at 52-55°C, stop the reaction after reacting for 48 hours, and cool the reaction solution to 30°C. The high performance liquid chromatography of reacting 12 hours and 36 hours is respectively as follows figure 1 and figure 2 shown. pass figure 1 and figure 2 compare and contrast image 3 , it can be seen that with the increase of enzymatic hydrolysis time, the concentration of icariin and other substrates relative to baohuoside I decreased, indicating that with the prolongation of enzymatic hydrolysis time, icariin and other substrates were converted into baohuoside I.

[0046] 2. Purification of ...

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Abstract

The preparation method provides a baohuoside-I preparation method which comprises the following steps: carrying out enzymolysis reaction of icariin under the action of pectinase to obtain crude baohuoside-I, and then carrying out two times of crystallization to obtain pure baohuoside-I. The mass yield of the baohuoside-I obtained by the method can reach more than 40% relative to 90% icariin, and the purity is above 99%.

Description

technical field [0001] The invention relates to a preparation method of baohuoside I, which belongs to the fields of food, health products, cosmetics and medicine. Background technique [0002] Baohuoside Ⅰ, also known as icariside II (Icariside II), is a new effective monomer obtained by enzymatic conversion of the main active ingredient icariin extracted from the Chinese herbal medicine Epimedium Herba. Its structural formula is as follows Shown in formula (I): [0003] [0004] Existing studies have shown that baohuoside I can improve cardiovascular function, regulate endocrine and enhance immunity. [0005] The preparation method of this compound is disclosed in 200780034447.9. In this method, icariin is used as a raw material, and an enzyme that can remove the glucose part or a microorganism that can produce the above-mentioned enzyme is used to catalyze hydrolysis. The reaction product is purified by silica gel column chromatography to obtain baohuoside Ⅰ Pure. D...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C12P19/60
Inventor 孟坤徐更张永圣刘丙征尚勇
Owner BEIJING SHENOGEN BIOMEDICAL
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