Method of extracting stigmasterol from mixed plant sterol

A technology of phytosterol and stigmasterol, which is applied in the direction of steroids and organic chemistry, can solve the problems of undisclosed high content, high requirements for reaction conditions, and low extraction efficiency, and achieve low product cost, low solvent toxicity, and selective good sex effect

Inactive Publication Date: 2002-10-16
武汉凯迪精细化工有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

But there is no disclosure to extract the method of high content bucket
Moreover, the method has high requirements on reaction conditions and long flow process; some equipment has large investment and low extraction efficiency.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1 basic operation:

[0020] 1. Add the mixed phytosterol to the reagent according to the mass volume ratio (m / V) of the mixed phytosterol to the solvent (m / v) 1:4.

[0021] 2. Seal and dissolve in a water bath at 70-75°C.

[0022] 3. After all the mixed phytosterols are dissolved, cool down in a water bath to 20-25°C. This process takes about 7-10 hours.

[0023] 4. Keep crystal growth at constant temperature for 12 hours.

[0024] 5. Insulation and decompression suction filtration. Collect the filter cake and filtrate.

[0025] 6. The crystal obtained by suction filtration was air-dried naturally, and the content of stigmasterol was detected.

[0026] 7. Carry out the next recrystallization according to the same material ratio, and repeat the operation steps 1-6 until the product reaches 85%. It usually takes 5 times.

[0027] 8. The filtrate is processed by low temperature or distillation at -10°C to recover sterols and solvents, which can be reused. ...

Embodiment 2

[0028] Embodiment 2: add 800ml analysis pure n-heptane in 200g phytosterol (purity 92.7%, stigmasterol content 27.5%): dichloroethane=630ml: 370ml mixed solvent in Erlenmeyer flask, press the mass volume of sterol and solvent Add the reagent at a ratio of 1:4, seal it, and dissolve it in a water bath at 75°C. After all the sterols were dissolved, the temperature was lowered in the water bath to 25°C and kept at a constant temperature for 12 hours. Insulate and filter under reduced pressure to collect the filter cake and filtrate. The crystals obtained by suction filtration were air-dried naturally, and the content of stigmasterol was detected. Carry out the next recrystallization according to the same material ratio. Recrystallized 5 times. The filtrate is processed at low temperature and distilled to recover sterols and solvents. The results of the five recrystallization experiments are as follows: 16.0.0 g of sterol was finally obtained, and the yield was 25.02%.

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PUM

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Abstract

The stigmasterol extracting process from mixed plant sterol is one stigmasterol enriching solvent process including the steps of water bath dissolution at 70-75 deg.c, cooling to 20-25 deg.c to crystallize for 12-24 hr, and heat insulating suction filtering. Mixed solvent is used including n-heptane and dichloroethane in the radio of 1 to 1-2, preferably 1 to 1.5-1.8. The ratio between mixed plant sterol and the solvent is 1 to 3-5, preferably 1 to 3.5-4.5. The said process is performed repeatedly for high stigmasterol content and the filtrate is low temperature treated at -10 deg.c to recover sterol and solvent.

Description

technical field [0001] The invention provides a method for extracting stigmasterol from mixed phytosterols. The invention belongs to the field of fine chemical industry. Background technique [0002] As a natural organic chemical, phytosterols are mostly derived from by-products of the vegetable oil industry. Among them, the most useful ones are vegetable oil derefining and deodorization distillate, alkali refining soapstock, distillation residue and other oil waste. Wherein the soybean oil deodorization distillate content is 9-22%, and the rapeseed oil deodorization distillate content is 24-25%. Most of the phytosterols are methyl-free sterols, the ratio is 50-97%, among which β-sitosterol, stigmasterol and campesterol account for more than half of the total sterols. At present, phytosterols mainly consist of β-sitosterol, stigmasterol, campesterol, and brassicasterol. These four phytosterols are all 4-methyl-free sterols, and the double bonds on ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
Inventor 王先宝耿建国谷文英盛漪刘长华
Owner 武汉凯迪精细化工有限公司
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