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Method for extracting stigmasterol from plant sterol

A technology for phytosterol and stigmasterol, applied in the directions of steroids, organic chemistry, etc., can solve the problems of low content and yield of stigmasterol, large environmental pollution, and high operation cost, and achieves improvement of purity and yield and reduction of production cost. , the effect of making full use of resources

Inactive Publication Date: 2005-05-18
ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
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AI Technical Summary

Problems solved by technology

[0003] Due to the extremely similar structure, it is difficult and cumbersome to separate and remove sitosterol and campesterol from phytosterols to obtain monomer stigmasterol with higher purity. There are generally three types of separation and purification of stigmasterol from phytosterols. Method: one is to use the double bond in the stigmasterol structural formula to form stigmasterol acetyl tetrabromide after bromination addition, and then obtain pure stigmasterol through a series of separation and treatment, but high temperature and high pressure environment will be used in the reaction. The operation cost is higher; the 2nd, can utilize chromatographic preparation technology, carry out separation and collection according to the difference of each sterol component retention time or Rf value, but with this method yield is less, and separation effect is not very satisfactory; 3rd, utilize organic solvent to carry out Multi-stage and step-by-step crystallization, and finally get stigmasterol with higher purity
The application number is 02115645.X, which discloses a method for separating and extracting stigmasterol from phytosterols with an organic solvent. The solvent multi-stage fractional crystallization method is adopted, and the selected organic solvent is a mixture of dichloroethane and n-heptane. In order to obtain high-purity stigmasterol from phytosterols, only multiple simple refining and separation treatments are carried out, which reduces the extraction yield. The stigmasterol content and yield obtained by this method are all low (the content is about 85%) , the yield is about 25%); and, the ethylene dichloride used is a chlorinated solvent, which has high toxicity and great environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The first step: phytosterol 100g (stigmasterol content 23.2%), in n-propanol 750ml 75 DEG C reflux dissolving 1hr, cool this solution to 20 DEG C crystallization, heat preservation crystal growth 15hr, rear filter, filter cake is vacuum-dried ( Vacuum degree -0.08~-0.09Mpa, temperature 40°C), after 5 hours, 48.5g of dry crystals (35.7% stigmasterol content) were obtained.

[0017] The second step: 48.5g of the phytosterol concentrate obtained in the first step is heated and dissolved in 245ml ethyl acetate, and the solution is incubated and grown for 14hr and then cooled to 40°C, and the deposited crystal is filtered, and the obtained crystal is used The same purification and separation conditions were used for 3 separation operations to obtain 3.5 g of stigmasterol (95.3% stigmasterol content), and the final yield after applying the mother liquor was 57.4%.

[0018] first step

Embodiment 2

[0020] The first step: 100g of phytosterol (stigmasterol 20.9%) is heated and dissolved in 800ml of absolute ethanol at 78°C, the solution is slowly cooled to 25°C and then crystallized, the crystal is grown for 12 hours and then filtered, and the obtained filter cake is vacuum-dried to obtain a concentrated plant Sterol 49.6g (stigmasterol content 41.2%).

[0021] The second step: heat and dissolve 49.6 g of the concentrated phytosterol obtained in the first step in 250 ml of isobutanol, then cool the solution to 40° C. to crystallize, grow crystals for 12 hours, and filter to obtain crystals. 3.9 g of stigmasterol (stigmasterol content: 95.4%) were obtained by performing two separation operations on the obtained crystals under the same purification and separation conditions.

[0022] The filtrate obtained in the first step and the second step crystallization, after measuring the content of stigmasterol wherein, can be mixed with the filter cake (the stigmasterol content is c...

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Abstract

The process of separating and purifying stigmasterol from plant sterol includes: the first step of adding solvent absolute ethyl alcohol, n-propanol or n-butanol, heating to dissolve, slowly lowering temperature to crystallize, filtering, centrifugally separating and vacuum drying; and the second step of adding separating solvent into the product of the first step, heating to dissolve, slowly lowering temperature to crystallize and filtering; with the separation capable of being repeated for 2 or 3 times. The present invention has separate material concentration and separation refining steps, and has greatly raised stigmasterol purity and yield and no environmental pollution.

Description

technical field [0001] The invention belongs to the field of fine chemical industry and relates to a method for separating and purifying stigmasterol from phytosterol. Background technique [0002] The phytosterol contained in plants is mainly a mixture of brassicasterol, campesterol, stigmasterol and sitosterol, which can be obtained in large quantities from the deodorized distillates of by-products in the deodorization process of oil in industry. Stigmasterol is used to synthesize adrenocortical hormone and luteinizing hormone medicines, and sitosterol and campesterol in phytosterols are worthless as raw materials for adrenal cortex hormone and luteinizing hormone medicine synthesis, if these worthless plants are not removed in advance The sterols, sitosterol, campesterol cause side effects and reaction disturbances, so they must be removed from the phytosterols. [0003] Due to the extremely similar structure, it is difficult and cumbersome to separate and remove sitoste...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J9/00
Inventor 许新德张定丰汪志明吕良伟
Owner ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
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