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Preparation technology for icariin

A technology of icariin and epimedium, which is applied in the field of preparing icariin, can solve the problems of complex process, high pressure on environmental protection, and low yield, and achieve simple production process, low pressure on environmental protection, and simple equipment Effect

Pending Publication Date: 2017-06-13
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this method, the adsorption capacity of macroporous resin to icariin is relatively small in a low-alcohol state, and there is leakage in the adsorption process, which easily leads to low yield; the polyamide separation and purification process is not easy due to the adoption of water-alcohol gradient elution. suitable for industrial production
The existing icariin preparation method has the problem of low product yield, and because the process is complicated, many highly toxic organic reagents are used, which is not suitable for industrialized large-scale production, and the pressure on environmental protection after amplification is also great

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] This embodiment includes the following steps:

[0020] (1) Extraction: Weigh 200 kg of Epimedium raw material (1.0% icariin content), pulverize, heat and reflux with steam to extract twice, add 3000 liters of 60% ethanol for the first time, extract for 3 hours, and extract for the second time Add 2000 liters of 60% ethanol, extract for 2 hours, combine the extracts, and concentrate the extracts under reduced pressure in vacuo.

[0021] (2) Extraction: After the extract is concentrated under reduced pressure to a volume of 400 liters, it is transferred to an extraction tank, 1200 liters of n-butanol is added, stirred for 5 minutes, and after standing for 2 hours, the n-butanol phase reclaims n-butanol to obtain n-butanol. Butanol extract 6535 grams, icariin content is 29.8%.

[0022] (3) Alcohol washing: add n-butanol extract to 100 liters of 50% ethanol, stir for 30 minutes, filter, and dry to obtain 3116 grams of icariin alcohol washing, with an icariin content of 60....

Embodiment 2

[0025] This embodiment includes the following steps:

[0026] (1) Extraction: Weigh 500 kg of Epimedium raw material (1.0% icariin content), pulverize, heat and reflux with steam to extract 3 times, add 15000 liters of 30% methanol for the first time, extract for 2 hours, and extract for the second time Add 10,000 liters of 30% methanol, extract for 2 hours, add 5,000 liters of 30% methanol for the third time, extract for 1 hour, combine the extracts, and concentrate the extracts under vacuum.

[0027] (2) Extraction: After the extract is concentrated under reduced pressure to a volume of 2500 liters, it is transferred to an extraction tank, 2500 liters of ethyl acetate is added, stirred for 5 minutes, and after standing for 3 hours, the ethyl acetate phase recovers ethyl acetate to obtain acetic acid The ethyl ester extract is 15985 grams, and the content of icariin is 30.5%.

[0028] (3) Alcohol washing: add the ethyl acetate extract to 80 liters of 85% methanol, stir for 3...

Embodiment 3

[0031] This embodiment includes the following steps:

[0032] (1) Extraction: Weigh 1000 kg of Epimedium raw material (1.0% icariin content), pulverize, heat and reflux with steam to extract 3 times, add 8000 liters of 80% methanol for the first time, extract for 3 hours, and extract for the second time Add 6000 liters of 80% methanol, extract for 2 hours, add 5000 liters of 80% methanol for the third time, extract for 1 hour, combine the extracts, and concentrate the extracts under vacuum.

[0033] (2) Extraction: After the extract is concentrated under reduced pressure to a volume of 1000 liters, it is transferred to an extraction tank, 5000 liters of ethyl acetate is added, stirred for 5 minutes, and after standing for 1 hour, the ethyl acetate phase recovers ethyl acetate to obtain acetic acid The ethyl ester extract is 32300 grams, and the content of icariin is 30.0%.

[0034] (3) Alcohol washing: Add the ethyl acetate extract to 970 liters of absolute ethanol, stir for ...

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Abstract

The invention relates to a preparation technology for icariin. The technology comprises the following steps: (1) extraction: crushing herba epimedii raw material, performing heating reflux extraction with alcoholic solution and concentrating an extracting solution; (2) extracting: extracting the concentrated extracting solution with n-butyl alcohol or ethyl acetate and recycling an organic solvent, thereby acquiring an extract containing icariin; (3) washing with alcohol: washing the extract containing icariin with absolute methanol, absolute ethyl alcohol, 40-95% ethyl alcohol or 30-95% methyl alcohol, washing the residual solid with alcohol and standing by for the next crystallizing; and (4) crystallizing: crystallizing the solid acquired in the previous step. The preparation technology provided by the invention is simple, the requirement for equipment is low, the product yield is high and the technology is suitable for industrial mass production.

Description

technical field [0001] The invention relates to a process for preparing icariin from epimedium. Background technique [0002] Icariin is the drying of Epimedium brevicornu Maxim of Berberidaceae, Epimedium sagittatum (Sieb.et Zucc.) Maxim, Epimedium pubescens Maxim or Epimedium koreanum Nakai Stem leaf extract. Molecular formula C 33 h 40 o 15 , molecular weight 676.65, CAS No. 489-32-7. Icariin has a variety of pharmacological effects, and its hydrolyzed product icariin has been approved as a first-class anti-cancer drug in traditional Chinese medicine, and has entered the fast-track approval process. In the study, another major achievement after artemisinin. However, the content of icariin in plants of the genus Epimedium is extremely low, and the feasible way to obtain icariin is to obtain icariin through hydrolysis of icariin. In the face of the research status and market demand of icariin, it is of great practical significance to study the preparation technology ...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08
CPCC07H1/08C07H17/07
Inventor 张贵民齐长鹏刘文平
Owner LUNAN PHARMA GROUP CORPORATION
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