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Method for extracting diosgenin from yellow ginger oil

A technology of diosgenin and turmeric oil, applied in the directions of steroids, organic chemistry, etc., can solve the problems of low recovery rate of active components, environmental pollution, complicated steps, etc., and achieves improved operability, reduced production cost, and simple operation. Effect

Active Publication Date: 2013-03-13
三原润禾生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The above enrichment and purification processes for diosgenin in turmeric oil all have the disadvantages of cumbersome steps and the use of a large amount of low-polarity solvents, causing environmental pollution, and the recovery rate of active ingredients is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) extract

[0031] The turmeric oil is extracted by stirring with ethyl acetate whose mass is 10 times, and the extraction temperature is 75°C to obtain the extract;

[0032] (2) Column chromatography

[0033] Concentrate the obtained extract to 1 / 5 of the original volume of the extract, and perform column chromatography. The column chromatography filler is polyamide and aluminum oxide (1:1), and the filler is 10 times the mass of the extract. Petroleum ether and chloroform Mixed solvent (13:2) for elution, TLC detection;

[0034] After the active ingredient is completely eluted as detected by TLC, the eluent containing the active ingredient is concentrated, placed for crystallization, suction filtered, and vacuum-dried for crystallization to obtain a diosgenin product.

[0035] The recovery rate of the effective components of the obtained product reaches 91%, and the content of saponin reaches 90.3%.

Embodiment 2

[0037] (1) extract

[0038] The turmeric oil is extracted by stirring with a mixed solvent of methanol with an amount 6 times its mass, and the extraction temperature is 100° C. to obtain an extract;

[0039] (2) Column chromatography

[0040] Concentrate the obtained extract to 1 / 8 of the original volume of the extract, apply column chromatography, the column chromatography filler is C18, the filler is 6 times the mass of the extract, eluted with acetone, and detected by TLC;

[0041] After the active ingredient is completely eluted as detected by TLC, the eluent containing the active ingredient is concentrated, placed for crystallization, suction filtered, and vacuum-dried for crystallization to obtain a diosgenin product.

[0042] The recovery rate of the effective components of the obtained product reaches 90%, and the content of saponin reaches 91.2%.

Embodiment 3

[0044] (1) extract

[0045] The turmeric oil is extracted by stirring with acetone three times its mass, and the extraction temperature is 50° C. to obtain an extract;

[0046] (2) Column chromatography

[0047] Concentrate the obtained extract to 1 / 10 of the original volume of the extract, and perform column chromatography. The column chromatography filler is silica gel, and the filler is 0.5 times the mass of the extract, and the mixed solvent of ethyl acetate and acetone (20:1) Carry out elution, TLC detects;

[0048] After the active ingredient is completely eluted as detected by TLC, the eluent containing the active ingredient is concentrated, placed for crystallization, suction filtered, and vacuum-dried for crystallization to obtain a diosgenin product.

[0049] The recovery rate of active ingredients in the obtained product reaches 92%, and the content of saponin reaches 90.5%.

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Abstract

The invention provides a method for extracting diosgenin from yellow ginger oil, which provides a convenient, quick and stable process route, optimizes extraction steps, reduces the production cost, enhances the operability and ensures favorable product quality and high recovery rate. The technical concept of the invention mainly comprises the following procedures: using ethanol, methanol, acetone, ethyl acetate and the like as primary extraction solvent, wherein most of impurities are removed after yellow ginger oil is subjected to ethanol extraction, but the properties of the residual impurity component are very similar to those of the product; and further purifying diosgenin through column chromatography, eluting with mixed petroleum ether and ethyl acetate, collecting fractions of effective components, concentrating, and standing to obtain the high-content diosgenin in one step without recrystallization, wherein organic solvent for eluting can be any one of petroleum ether, ethyl acetate, chloroform and acetone alone or can be in other mixed eluting matching modes.

Description

technical field [0001] The invention relates to a method for extracting diosgenin, in particular to a method for separating and extracting diosgenin from turmeric oil. Background technique [0002] Yellow ginger (Dioscorea zingibernsis C.H.wright), scientific name Dioscorea zingibernsis, also known as fire head root, pillow root, etc., is a perennial winding herbaceous vine plant of the genus Dioscrea. Jiangxi, Gansu, Sichuan, Yunnan, Guizhou and other places. [0003] Diosgenin (Diosgenin), chemical name: isospiro-5-en-3β-ol, molecular formula: C 27 h 42 o 3 , white or yellowish flaky or needle-like crystals, easily soluble in gasoline, ethanol, chloroform and other organic solvents, insoluble in water. Dioscin is an important basic raw material and starting intermediate for the production of steroid hormone drugs. The main component of drugs such as cardiac glycosides and progesterone, from which almost all steroid hormone drugs can be synthesized. Steroid hormone dr...

Claims

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Application Information

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IPC IPC(8): C07J71/00
Inventor 杨军仁王晓莹肖红
Owner 三原润禾生物科技有限公司
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