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Purifying method of ticogenin crude product

A technology of sisal saponin and purification method, applied in the direction of steroids, organic chemistry, etc., can solve the problems of sisal saponin not being recyclable, waste, etc., and achieve production and quality control, short route, purity and yield high effect

Inactive Publication Date: 2014-10-22
广西众益生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method is that the crude sisal saponin is dissolved in alcohol, decolorized, filtered, and the filtrate is concentrated, cooled, left to stand for crystallization, and filtered to obtain sisal saponin and mother liquor with higher content. Although this method can obtain High-content products, but the yield of sisal saponin is generally only 70%-80%, some sisal saponin and impurities are dissolved into the mother liquor, and need to be recrystallized 2-3 times again, and the final mother liquor is about 8-10% of sisal saponin cannot be recovered, and it is discharged together with impurities, resulting in huge waste

Method used

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  • Purifying method of ticogenin crude product

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Effect test

Embodiment 1

[0040] The purification method of sisal saponin crude product of the present invention, comprises the steps:

[0041]A, be 40% ethanol as cleaning agent with 640g mass concentration, clean 80g sisal saponin content and be the sisal saponin crude product of 65%, constantly stir and dissolve impurity, filter, obtain filtrate 1 and filter cake 1, filter cake 1 Heat and dry at 100°C for 5 hours to obtain the sisal saponin product, weighing 61.42g and detecting that the sisal saponin content is 75.43%;

[0042] B. Cool the filtrate 1 to 0°C, let it stand still to precipitate impurities, and filter to obtain filtrate 2 and 30.00g of impurity filter cake 2;

[0043] C, the filtrate 2 is used as a cleaning agent for the cleaning of a new batch of sisal saponin crude product, and steps A and B are repeated.

[0044] Also includes the following steps:

[0045] D, repeat step C, successively wash and purify multiple batches of sisal saponin crude product. The average content of sisal ...

Embodiment 2

[0049] The purification method of sisal saponin crude product of the present invention, comprises the steps:

[0050] A, be 60% ethanol as cleaning agent with 800g mass concentration, clean 80g sisal saponin content and be the sisal saponin crude product of 80%, constantly stir and dissolve impurity, filter, obtain filtrate 1 and filter cake 1, filter cake 1 Heat and dry at 100°C for 5 hours to obtain the sisal saponin product, weighing 60.12g, and the sisal saponin content is 93.08%;

[0051] B. Cool the filtrate 1 to 5°C, let stand to precipitate impurities, and filter to obtain filtrate 2 and 24.32g impurity filter cake 2;

[0052] C, the filtrate 2 is used as a cleaning agent for the cleaning of a new batch of sisal saponin crude product, and steps A and B are repeated.

[0053] Also includes the following steps:

[0054] D, repeat step C, successively wash and purify multiple batches of sisal saponin crude product. The average content of sisal saponin products is 92.18...

Embodiment 3

[0058] The purification method of sisal saponin crude product of the present invention, comprises the steps:

[0059] A, be 70% ethanol as cleaning agent with 1000g mass concentration, clean 80g sisal saponin content and be on the filter that the sisal saponin crude product of 80% is placed, add cleaning agent continuous cleaning and filtration, filter and remove impurity, obtain Filtrate 1 and filter cake 1, filter cake 1 was heated and dried at 100°C for 5 hours to obtain the sisal saponin product, weighing 58.67g, and the content of sisal saponin was 94.36% in detection;

[0060] B. Cool the filtrate 1 to 10°C, let stand to precipitate impurities, and filter to obtain filtrate 2 and 22.94g impurity filter cake 2;

[0061] C, the filtrate 2 is used as a cleaning agent for the cleaning of a new batch of sisal saponin crude product, and steps A and B are repeated.

[0062] Also includes the following steps:

[0063] D, repeat step C, successively wash and purify multiple bat...

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Abstract

A purifying method of a ticogenin crude product is disclosed. The purifying method includes steps of: A) cleaning the ticogenin crude product by adopting ethanol having a concentration of 40-90% as a cleaning agent, dissolving impurities and filtering to obtain a filtrate 1 and a filter cake 1, drying the filter cake 1 to obtain a ticogenin product; B) cooling the filtrate 1 to 0-50 DEG C, allowing the filtrate 1 to stand to precipitate the impurities, and filtering to obtain a filtrate 2 and an impurity filter cake 2; and C) repeating steps A) and B) by adopting the filtrate 2 as a cleaning agent for cleaning of a new batch of the ticogenin crude product. The purifying method has characteristics of short and simple process, convenient operation, high ticogenin purity and yield, low solvent consumption, good economic benefit and environmental benefit, and suitability for continuous industrial production.

Description

technical field [0001] The invention relates to a method for purifying a crude product, in particular to a method for purifying a crude product of sisal saponin. Background technique [0002] Sisal saponin, also known as sisal saponin, tecoginine, etc., has a complete steroidal skeleton structure and good biological activity. It is a very tight hormone drug raw material in the market and can be used to synthesize more than 200 steroids. Body hormone drugs, such as: adrenocortical hormone, sex hormone and anabolic hormone drugs, known as "medicine gold" and "mother of hormones". [0003] Sisal saponin is generally derived from sisal juice or sisal paste formed by the fermentation of juice. Sisal saponin is extracted from sisal, and the juice is usually squeezed from the sisal residue after defiberization, and the juice is placed in a sedimentation tank. Naturally ferment for two weeks, filter out the precipitate, and dry it to obtain sisal paste. Use acid to hydrolyze the si...

Claims

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Application Information

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IPC IPC(8): C07J71/00
Inventor 王俊覃佑康阮恒黄转香廖青黄尚顺李华锋秦高雄
Owner 广西众益生物科技有限公司