Method for extracting and preparing 4,4'-dimethylsterol from shea nut butter

A technology of dimethyl sterol and shea butter, applied in the field of separation engineering, can solve the problems of low product yield, cumbersome process, complicated process, etc., and achieve the effect of high purity, simple process and high extraction efficiency

Active Publication Date: 2019-03-29
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, most of the sterols prepared at home and abroad are 4-methyl-free sterols, which have many defects such as complex process, cumbersome process, high energy consumption, and low product yield. Sterols have not been reported in the literature
Shea butter mainly contains triglycerides, free fatty acids and 4,4'-dimethyl sterol esters, etc. The properties are relatively close, and it is difficult to separate them by pure physical methods

Method used

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  • Method for extracting and preparing 4,4'-dimethylsterol from shea nut butter
  • Method for extracting and preparing 4,4'-dimethylsterol from shea nut butter
  • Method for extracting and preparing 4,4'-dimethylsterol from shea nut butter

Examples

Experimental program
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Effect test

Embodiment 1

[0034] (1) Take 30 grams of shea butter, put it into a flask for saponification, add 200 mL of potassium hydroxide ethanol solution with a concentration of 1 mol / L, reflux and saponify at 105° C. for 1 hour, and collect the oily liquid after saponification;

[0035] (2) Add 120mL of n-hexane to the oily liquid after saponification, separate layers, let go of the lower liquid, take the upper liquid organic layer, wash twice with 40°C warm water 240mL, and separate the liquid to obtain The feed liquid of base sterol;

[0036] (3) Distill the feed solution containing 4,4'-dimethylsterol at 37°C and -0.09MPa to remove n-hexane to obtain 2.3 grams of 4,4'-dimethylsterol enrichment;

[0037] (4) Add 2.3 grams of 4,4'-dimethyl sterol enrichment to 23 mL of ethanol and raise the temperature to 60°C to dissolve, then cool the solution to 25°C to crystallize, grow crystals for 8 hours, and separate to obtain 4,4' - Dimethyl sterol crystals, yield 46.9%.

[0038] figure 1 It is the no...

Embodiment 2

[0042] (1) Take 30 grams of shea butter, put it into a flask for saponification, add 200 mL of potassium hydroxide ethanol solution with a concentration of 1 mol / L, reflux and saponify at 105° C. for 1 hour, and collect the oily liquid after saponification;

[0043] (2) Add 250mL of petroleum ether to the oily liquid after saponification, separate layers, let go of the lower liquid, take the upper liquid organic layer, wash twice with 55°C warm water 250mL, and separate the liquid to obtain The feed liquid of base sterol;

[0044] (3) Evaporate the feed liquid containing 4,4'-dimethyl sterol at 37°C and -0.09 MPa to remove petroleum ether to obtain 3.2 grams of 4,4'-dimethyl sterol enrichment;

[0045] (4) Add 2.3 grams of 4,4'-dimethyl sterol enrichment into 50 mL of acetone and heat up to 65°C to dissolve, then cool the solution to 30°C to crystallize, grow crystals for 10 hours, and separate to obtain 4,4' - Dimethyl sterol crystals, yield 67.2%. image 3 For the prepared...

Embodiment 3

[0047] (1) Take 30 grams of shea butter, put it into a flask for saponification, add 200 mL of potassium hydroxide ethanol solution with a concentration of 1 mol / L, reflux and saponify at 105° C. for 1 hour, and collect the oily liquid after saponification;

[0048] (2) Add 250mL of n-hexane to the oily liquid after saponification, separate layers, let go of the lower liquid, take the upper liquid organic layer, wash twice with 300mL of warm water at 85°C, and separate liquids to obtain The feed liquid of base sterol;

[0049] (3) Evaporate the feed solution containing 4,4'-dimethyl sterol at 37°C and -0.09 MPa to remove n-hexane to obtain 4.2 grams of 4,4'-dimethyl sterol enrichment;

[0050] (4) Add 4.2 grams of 4,4'-dimethyl sterol enrichment to 100 mL of a mixed solution of ethanol and isopropanol (1:2, v / v) and heat up to 75°C to dissolve, and then the solution Cool to 25°C for crystallization, grow the crystals for 12 hours, and obtain 4,4'-dimethyl sterol crystals with...

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Abstract

The invention discloses a method for extracting and preparing 4,4'-dimethylsterol from shea nut butter. The method comprises the following steps: taking shea nut butter as a raw material, adding a potassium hydroxide ethanol solution, carrying out saponification treatment, and a collecting saponified oily liquid; adding a solvent into the saponified oily liquid, performing layering, taking out anorganic layer, adding water for washing, and performing liquid separation to obtain a feed liquid containing 4,4'-dimethylsterol; evaporating the feed liquid containing the 4,4'-dimethylsterol at 37 DEG C under the condition of -0.09 MPa, and removing the solvent to obtain an 4,4'-dimethylsterol-enriched product; and adding a solvent into the 4,4'-dimethylsterol-enriched product, heating the 4,4'-dimethylsterol-enriched product to 60-85 DEG C for dissolving, and performing cooling and crystallizing to obtain a pure 4,4'-dimethylsterol product. The method has the advantages of simple process steps, easy solvent recovery, low energy consumption, high product purity and extraction efficiency, and capability of industrial production.

Description

technical field [0001] The invention belongs to the technical field of separation engineering, and in particular relates to a method for extracting and preparing 4,4'-dimethyl sterol from shea butter. Background technique [0002] 4,4'-Dimethyl sterol is a component in the unsaponifiable matter of vegetable oil. For most vegetable oils, the content of 4-non-methyl sterol (stigmasterol, campesterol, sitosterol) in the unsaponifiable matter higher, and lower 4,4'-dimethylsterol content. The content of unsaponifiable matter in shea butter is as high as 10%, and the main content is 4,4'-dimethyl sterol. Shea butter can be used as a new food raw material, and the unsaponifiable matter resource after saponification of shea butter can be used to extract 4,4'-dimethyl sterol. The 4,4'-dimethyl sterols in shea butter include lupeol, α-amyresinol, β-amyresinol, butyryl cetyl alcohol, and mannisol. Many studies have shown that the 4,4'-dimethyl sterol contained in shea butter has th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K36/185A61P3/04A61P25/16A61P25/20A61P29/00A61K131/00
CPCA61K36/185A61K2236/333A61P3/04A61P25/16A61P25/20A61P29/00
Inventor 常明张涛王兴国金青哲刘睿杰黄健花
Owner JIANGNAN UNIV
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