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Production process of medicinal gossypol acetic acid

A technology of gossypol acetate and production process, which is applied in the field of production of medicinal gossypol acetate, can solve the problems of high price, harm to human body, low boiling point, etc., and achieve the effects of increased yield, high Buddha point, and low price

Inactive Publication Date: 2008-06-18
JINAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

All need to use a large amount of acetone, diethyl ether, chloroform, aniline etc., so far all industrialized technology basic parts need to use aniline, these solvents are all poisonous even highly toxic, simultaneously boiling point is low, price is high, is unfavorable for suitability for industrialized production; There is a small amount of aniline remaining in the product, which is harmful to the human body
[0004] The Chinese invention patent with the patent number ZL 200410025855.6 discloses a production method of gossypol acetate raw material, which uses acetone heat reflux-acetic acid recrystallization method to produce gossypol acetate raw material in large quantities and with high efficiency; the patent number is ZL The Chinese invention patent of 85108568 discloses an acetone-water release process method to prepare gossypol acetate, which uses water to dilute the acetone aqueous solution to extract the cotton kernel, so that the gossypol is folded out, and then electrolyte is added to break the emulsion, and the crystal is grown statically , separation, washing and refining to obtain gossypol acetate that meets quality standards: the above-mentioned two disclosed patents all need to use a large amount of acetone, which is poisonous and has low boiling point and high price, which is not conducive to industrial production

Method used

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  • Production process of medicinal gossypol acetic acid
  • Production process of medicinal gossypol acetic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Put 1 kg of cottonseed into a 10-liter Erlenmeyer flask, extract with 5 liters of ethanol, stir for 3-4 hours, and extract three times at an extraction temperature of 60°C. The residue was removed by centrifugation, concentrated and then applied to a macroporous resin chromatography column (AB-8), gradient eluted with 50%, 60%, 70%, and 80% ethanol respectively, and the eluate of gossypol was collected.

[0025] Concentrate the collected gossypol eluate to 1 L, and add 0.05 L of glacial acetic acid for acidification. Store at 6°C for 10 hours. After centrifugation, the filter cake is placed in a vacuum drying oven, controlled at a temperature of 50-60° C., and dried for 3 hours. The crude product of gossypol acetate was obtained.

[0026] Take out the filter cake, add ether until completely dissolved, add dropwise glacial acetic acid until yellow turbidity appears, put it in the freezer and let it stand at 10°C for 4 hours. Suction filtration, washing with petroleum ...

Embodiment 2

[0028] Put 10kg of cottonseed into a 100-liter reactor, extract with 50 liters of ethanol, stir for 3-4 hours, and extract three times at a temperature of 50-60°C. The residue was removed by centrifugation, concentrated and then applied to a macroporous resin chromatography column (X-5), gradient eluted with 50%, 60%, 70%, 80% ethanol respectively, and the gossypol eluate was collected.

[0029] The collected gossypol eluate was concentrated to 15 liters and acidified by adding glacial acetic acid (0.75 liters). Store at 8°C for 12 hours. After centrifugation, the filter cake is placed in a vacuum drying oven, controlled at a temperature of 50-60° C., and dried for 2 hours. The crude product of gossypol acetate was obtained.

[0030] Take out the filter cake, add ether until completely dissolved, add dropwise glacial acetic acid until yellow turbidity appears, and put it in the freezer at 8°C for 3 hours. Suction filtration, washing with petroleum ether, vacuum drying of th...

Embodiment 3

[0032] Put 50kg of cottonseed into a multifunctional extraction tank, extract with 250 liters of ethanol, stir for 3-4 hours, and extract three times at an extraction temperature of 50°C. The residue was removed by centrifugation, concentrated and then applied to a macroporous resin chromatography column (AB-8), gradient eluted with 50%, 60%, 70%, and 80% ethanol respectively, and the eluate of gossypol was collected.

[0033] Concentrate the collected gossypol eluate to 60 liters, and add 3 liters of glacial acetic acid for acidification. Store at 5°C for 10 hours. After centrifugal separation, the filter cake was placed in a vacuum drying oven at a controlled temperature of 50° C., and dried for 2 hours. The crude product of gossypol acetate was obtained.

[0034] Take out the filter cake, add acetone until it is completely dissolved, add dropwise glacial acetic acid until yellow turbidity appears, and put it in a freezer at 8°C for 3 hours. Suction filtration, washing wi...

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Abstract

The invention discloses a production technology for medicinal gossypol acetate. The technology includes (1) crushing the cotton seeds, extracting with ethanol, centrifugating and separating to remove residues, eluting through chromatography column with ethanol, and collecting the eluate; (2)adding acetic acid for acidification until no longer producing more precipitation, centrifugating and separating the acidified liquid, and drying the cake in a vacuum oven to obtain a crude gossypol acetate; and (3) adding ethyl ether or acetone in the crude gossypol acetate until dissolving wholly, dropping glacial acetic acid until yellow turbidity, standing and filtering, washing with petroleum ether, and vacuum-drying the cake to obtain the refined gossypol acetate. The invention has the advantages of increased yield of gossypol acetate, high purity and non-use of highly toxic acid aniline, so that the products can be used to pharmaceuticals.

Description

technical field [0001] The invention relates to a process for producing medicinal gossypol acetate. Background technique [0002] my country is a big cotton planting country, with an annual output of about 8 million tons of cottonseed. Gossypol is toxic and needs to be removed when cottonseed is further processed for cottonseed oil and feed. Gossypol acetate is a compound with a wide range of pharmacological effects: it has anti-fertility, anti-inflammation, anti-virus, and anti-parasitic effects; Cancer and certain gynecological diseases such as uterine fibroids, endometriosis, and functional bleeding are all curative. According to the latest market conditions (early September 2006), the selling price of gossypol acetate that meets the national standard (colorimetric method 97%) has reached about 60,000 yuan / kg. It can be seen that extracting and refining gossypol from cottonseed can realize the comprehensive utilization of cottonseed, greatly increase its added value, a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/57C07C45/78
Inventor 胡长鹰徐德平
Owner JINAN UNIVERSITY