Method for preparing silybin

A technology for silibinin and silymarin, which is applied to the field of extraction and purification of silibinin, can solve the problems of high production cost, harm to the human body, large dosage, etc., achieves low energy consumption, improves product purity and toxicity low effect

Inactive Publication Date: 2010-09-01
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] There are many silymarin manufacturers in my country, but the technology is relatively backward
The preparation of silybin is usually extracted by ethyl acetate method, which has less silybin content and low yield [Shi Jinsong, Sun Dafeng, Gu Gongping. Improvement and discussion of silymarin extraction process[J], China Wild Plant Resources. 2006, 12(25): 52-54]
Zhang Shouqin et al. "Research on the Extraction of Silymarin at Normal Temperature and Ultra-high Pressure" reported a method for extracting silymarin using ultra-high pressure technology. The pressure conditions of this method have high requirements on the extractor, which greatly increases the investment cost; Silymarin Technology” reported a method for preparing silibinin by extracting with acetone and degreasing petroleum ether. In this method, after degreasing, the oil and fat components will affect the extraction effect, increase the extraction time, and petroleum ether is more toxic , is unfavorable for expanding production; and for example Chinese patent CN101260105 "A kind of extraction method of silybin" has reported a kind of method starting from silymarin, ethanol reflux extraction to prepare silybin, and this method uses a lot of ethanol and consumes a lot of energy , the production cost is high; for another example, Wang Cuiyan et al. "Research on the Extraction Method of Silybin" described two methods for preparing silibinin, reflux extraction and ultrasonic extraction. The degreasing all uses petroleum ether and the consumption is large, which is used for the production of silybin. very dangerous

Method used

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  • Method for preparing silybin

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Experimental program
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Effect test

Embodiment 1

[0033] The milk thistle seeds were pulverized into 20 meshes, 10 kg (0.96% of silybin content) was added to 80 L of n-hexane, defatted 3 times, each time for 1.5 hours, and the dregs were filtered out as defatted coarse material. Add 40L of 40% dilute ethanol to the degreased crude material for reflux extraction three times, combine the extracts, concentrate under reduced pressure until there is no alcohol smell, add 30L of ethyl acetate for extraction, and obtain the extract. The extract was mixed with 200-300 mesh silica gel, and then put on a 5L silica gel column, and eluted sequentially with benzene, 4:1 and 2:1 (v / v) benzene-ethyl acetate at a flow rate of 5L / h. Take the colorless effluent as the end point, collect 2:1 (v / v) benzene-ethyl acetate eluent in sections of 200ml each, and detect with ultraviolet light after the elution is completed, and the 13~ The 21 eluents were combined, and the solvent was recovered under reduced pressure to obtain 113 g of extract. Add 8...

Embodiment 2

[0035] The milk thistle seeds were pulverized into 40 meshes, 10 kg (0.99% of silybin content) was added to 90 L of n-hexane, defatted 3 times, each time for 1.5 hours, and the dregs were filtered out as defatted coarse material. Add 50L of 45% dilute ethanol to the degreased crude material for reflux extraction for 3 times, combine the extracts, concentrate under reduced pressure until there is no alcohol smell, add 35L of ethyl acetate for extraction, and obtain the extract. The extract was mixed with 200-300 mesh silica gel, then put on a 5L silica gel column, and eluted with benzene, 5:1 and 1:1 (v / v) benzene-ethyl acetate successively at a flow rate of 5L / h. Respectively take the colorless effluent as the end point, collect 1:1 (v / v) benzene-ethyl acetate eluent in sections of 200ml each, and detect with ultraviolet light after the elution is completed, and the 13~ The 21 eluents were combined, and the solvent was recovered under reduced pressure to obtain 119 g of extrac...

Embodiment 3

[0037] The milk thistle seeds were pulverized into 40 meshes, 10 kg (0.98% of silybin content) was added to 100 L of n-hexane, defatted 3 times, each time for 2 hours, and the dregs were filtered out as defatted coarse material. Add 55L of 50% dilute ethanol to the degreased crude material for reflux extraction twice, combine the extracts, concentrate under reduced pressure until there is no alcohol smell, add 35L of ethyl acetate for extraction, and obtain the extract. The extract was mixed with 200-300 mesh silica gel, then put on a 5L silica gel column, and eluted sequentially with benzene, 6:1 and 2:1 (v / v) benzene-ethyl acetate at a flow rate of 5L / h. Take the colorless effluent as the end point, collect 2:1 (v / v) benzene-ethyl acetate eluent in sections of 200ml each, and detect with ultraviolet light after the elution is completed, and the 13~ The 21 eluents were combined, and the solvent was recovered under reduced pressure to obtain 124 g of extract. Add 1000ml of 60...

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Abstract

The invention relates to a method for preparing silybin. The method comprises the following process steps: crushing silybin seeds into 20 to 40 meshes, and degreasing the crushed silybin seeds thrice by using n-hexane; refluxing and extracting degreased coarse materials by using dilute ethanol; concentrating the extract under reduced pressure till the extract has no ethanol smell, extracting the concentrate by using ethyl acetate, stirring and drying ester phase and silica gel, then injecting a dried product to a column, eluting the dried product by using benzene or benzene-ethyl acetate, collecting the elute by sections, combining the elute to obtain main elute component of the silybin, concentrating the elute under reduced pressure, dissolving the elute in ethanol solution, adding active carbon into the solution, stirring the solution, decolorizing the solution for 0.5 to 1 hour, filtering the active carbon from the decolorized solution, concentrating the decolorized solution under reduced pressure to 40 to 60 percent of the primary volume, cooling the concentrate to separate out crystals, crystallizing the crystals by using hot ethanol, and repeating the crystallization step for 2 to 4 times to obtain the silybin. The method for producing the silybin has the advantages of simple process, low solvent toxicity, low production cost, and easy realization of industrialization.

Description

Technical field: [0001] The invention relates to an extraction and purification process of silybin, in particular to a method for extracting and purifying silybin by using silica gel chromatography and crystallization. Background technique: [0002] Silybin [0003] Alias: Yiganling, Milk Thistle, Sirimilin [0004] Chemical name: 2,3-Dihydro-3-(4-hydroxy-3-methoxyphenyl)-2-(hydroxymethyl)-6-(3,5,7-trihydroxy-4-oxobenzopyran-2-yl)benzodioxin [0005] Molecular formula and molecular weight: C 25 h 22 o 10 , 482.44 [0006] [0007] Properties: off-white crystalline powder. Odorless, slightly bitter taste, hygroscopic. Soluble in acetone, ethyl acetate, methanol, ethanol, slightly soluble in chloroform, almost insoluble in water. Monohydrate (methanol-water), mp.180°C; anhydrous, mp.158°C (decomposition at 180°C). [0008] Pharmacological action: silibinin has the obvious effect of protecting and stabilizing liver cells, and is used to treat acute and chronic hepat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D407/04
Inventor 刘东锋张翼杨成东
Owner NANJING ZELANG MEDICAL TECH
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