CN109528784B - Method for extracting and preparing 4,4' -dimethyl sterol from shea butter - Google Patents
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Abstract
The invention discloses a method for extracting and preparing 4,4' -dimethyl sterol from shea butter, which comprises the steps of taking shea butter as a raw material, adding a potassium hydroxide ethanol solution for saponification, and collecting saponified oily liquid; adding a solvent into the saponified oily liquid, layering, taking out an organic layer, adding water for washing, and separating to obtain a feed liquid containing 4,4' -dimethyl sterol; evaporating feed liquid containing 4,4 '-dimethyl sterol at 37 ℃ and under the pressure of-0.09 MPa, and removing a solvent to obtain an enrichment substance of 4,4' -dimethyl sterol; adding a solvent into the enriched 4,4 '-dimethyl sterol, heating to 60-85 ℃ for dissolving, cooling and crystallizing to obtain a pure 4,4' -dimethyl sterol product. The method has the advantages of simple process steps, easy solvent recovery, low energy consumption, high product purity and extraction efficiency, and can be used for industrial production.
Description
Technical Field
The invention belongs to the technical field of separation engineering, and particularly relates to a method for extracting and preparing 4,4' -dimethyl sterol from shea butter.
Background
4,4 '-dimethyl sterol is a component of unsaponifiable vegetable oils, and for most vegetable oils the unsaponifiable matter contains a high content of 4-methyl free sterols (stigmasterol, campesterol, sitosterol) and a low content of 4,4' -dimethyl sterol. The content of unsaponifiable matter in the shea butter is up to 10 percent, and the shea butter basically takes 4,4' -dimethyl sterol as the main component. The Shea butter can be used as new food material, and the unsaponifiable matter resource of Shea butter after saponification can be used for extracting 4,4' -dimethyl sterol. The 4,4' -dimethyl sterol in shea butter comprises lupeol, alpha-resinol, beta-resinol, butyryl cetanol, and mannich. Many researches show that the 4,4 '-dimethyl sterol contained in the shea butter has the effects of improving obesity, Parkinson's disease, sleep disorder, analgesia and the like. At present, the application of shea butter is focused on the cosmetic field, and related research and application in the fields of functional foods, medicines and the like are gradually rising.
At present, most of sterols prepared at home and abroad are 4-methyl-free sterols, and the defects of complex process, fussy flow, high energy consumption, low product yield and the like exist, and no literature report is found on the extraction and preparation of 4,4' -dimethyl sterol from vegetable oil. The shea butter mainly contains components such as triglyceride, free fatty acid and 4,4 '-dimethyl sterol ester, and the triglyceride and the 4,4' -dimethyl sterol ester have relatively close physical properties such as boiling point and solubility, and are difficult to separate by a simple physical method.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made in view of the above-mentioned technical drawbacks.
Therefore, as one aspect of the invention, the invention overcomes the defects of long preparation process, large equipment investment, energy waste and the like in the prior art, thereby reducing the production cost and improving the economic benefit, and provides a method for extracting and preparing 4,4' -dimethyl sterol from shea butter.
In order to solve the technical problems, the invention provides the following technical scheme: a method for extracting and preparing 4,4' -dimethyl sterol from shea butter is characterized in that: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
taking shea butter as a raw material, adding a potassium hydroxide ethanol solution for saponification, and collecting saponified oily liquid;
adding a solvent into the saponified oily liquid, layering, taking out an organic layer, adding water for washing, and separating to obtain a feed liquid containing 4,4' -dimethyl sterol;
evaporating feed liquid containing 4,4 '-dimethyl sterol at 37 ℃ and under the pressure of-0.09 MPa, and removing a solvent to obtain an enrichment substance of 4,4' -dimethyl sterol;
adding a solvent into the enriched 4,4 '-dimethyl sterol, heating to 60-85 ℃ for dissolving, cooling and crystallizing to obtain a pure 4,4' -dimethyl sterol product.
The method for extracting and preparing 4,4' -dimethyl sterol from shea butter is characterized by comprising the following steps: the method is characterized in that shea butter is used as a raw material, a potassium hydroxide ethanol solution is added for saponification, and the saponification is carried out on shea butter, wherein the saponification is carried out by the following raw materials in g: measured by mL, shea butter raw material: the potassium hydroxide ethanol solution was 3: 20; the concentration of the potassium hydroxide ethanol solution is 1 mol/L.
The method for extracting and preparing 4,4' -dimethyl sterol from shea butter is characterized by comprising the following steps: and (3) performing saponification treatment, wherein the saponification temperature is 105 ℃, and the saponification time is 1 h.
The method for extracting and preparing 4,4' -dimethyl sterol from shea butter is characterized by comprising the following steps: adding a certain amount of solvent into the saponified oily liquid to extract 4,4' -dimethyl sterol, wherein the solvent is one of n-hexane, petroleum ether, diethyl ether and dichloromethane; in mL: g, solvent: the shea butter raw materials are 4-10: 1.
the method for extracting and preparing 4,4' -dimethyl sterol from shea butter is characterized by comprising the following steps: and taking out the organic layer, adding water for washing, and separating liquid to obtain a feed liquid containing 4,4' -dimethyl sterol, wherein the water is added for washing, the washing temperature is 40-85 ℃, and the volume ratio of water to the organic layer is 1-4: 1, the number of water washes was 2.
The method for extracting and preparing 4,4' -dimethyl sterol from shea butter is characterized by comprising the following steps: adding a solvent into the enriched 4,4 '-dimethyl sterol, heating to 60-85 ℃ for dissolving, cooling and crystallizing to obtain a pure 4,4' -dimethyl sterol product, wherein the solvent is one or two of acetone, butanone, n-butanol, isopropanol, isobutanol and ethanol.
The method for extracting and preparing 4,4' -dimethyl sterol from shea butter is characterized by comprising the following steps: and cooling and crystallizing at the crystallization temperature of 25-45 ℃ for 8-16 h.
The method for extracting and preparing 4,4' -dimethyl sterol from shea butter is characterized by comprising the following steps: adding a solvent into the enriched 4,4 '-dimethyl sterol, heating to 60-85 ℃, dissolving, cooling and crystallizing to obtain a pure 4,4' -dimethyl sterol product, wherein the weight ratio of g: mL, enrichment of 4,4' -dimethyl sterol: the solvent is 1: 10 to 30.
The method for extracting and preparing 4,4' -dimethyl sterol from shea butter is characterized by comprising the following steps: the 4,4' -dimethyl sterol comprises lupeol, butyryl cetanol and balsamic alcohol.
The invention has the beneficial effects that:
1. the invention combines a chemical method and a physical method, overcomes the characteristics of similar physical properties such as boiling point, solubility and the like between triglyceride and 4,4' -dimethyl sterol ester, and improves the product yield and purity, wherein the triglyceride and the 4,4' -dimethyl sterol ester are respectively converted into free fatty acid and free 4,4' -dimethyl sterol by chemical saponification reaction, the polarity difference between the triglyceride and the free 4,4' -dimethyl sterol is enhanced, and the technical difficulty that the properties such as boiling point, solubility and the like are similar when the triglyceride and the 4,4' -dimethyl sterol ester are directly separated from the shea butter is avoided. In addition, saponification is beneficial to the subsequent physical crystallization, separation and purification of 4,4' -dimethyl sterol, compared with the prior art, the method for extracting and preparing 4,4' -dimethyl sterol from grease for the first time has the advantage that the obtained 4,4' -dimethyl sterol has high purity and can be directly used in the fields of medicines, chemical engineering and the like.
2. The method has the advantages of simple process flow, low requirement on equipment, capability of quickly realizing extraction and preparation of the high-purity 4,4' -dimethyl sterol, suitability for industrial production, capability of recycling the used solvent, full utilization of resources, low energy consumption and great reduction of production cost.
3. The method has high extraction efficiency, and is suitable for refined shea butter or shea butter with wide adaptability to the raw material shea butter, poor quality or longer storage time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is a normal phase high performance liquid chromatogram of 4-methylsterol-free (stigmasterol) and 4,4' -dimethylsterol (lupeol) standards.
FIG. 2 is a high performance liquid chromatogram of 4,4' -dimethyl sterol obtained from the preparation of Shea butter by extraction in example 1.
FIG. 3 is a high performance liquid chromatogram of 4,4' -dimethyl sterol obtained from the preparation of Shea butter by extraction in example 2.
FIG. 4 is a high performance liquid chromatogram of 4,4' -dimethyl sterol obtained from the preparation of Shea butter by extraction in example 3.
FIG. 5 is a reversed-phase high performance liquid chromatogram of the pure 4,4' -dimethylsterol obtained in example 3.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
(1) Taking 30 g of shea butter, filling the shea butter into a flask, saponifying, adding 200mL of 1mol/L potassium hydroxide ethanol solution, refluxing and saponifying at 105 ℃ for 1h, and collecting saponified oily liquid;
(2) adding 120mL of normal hexane into the saponified oily liquid, layering, discharging the lower layer of liquid, taking the organic layer of the upper layer of feed liquid, washing twice with 240mL of warm water at 40 ℃, and separating liquid to obtain feed liquid containing 4,4' -dimethyl sterol;
(3) the feed liquid containing 4,4 '-dimethyl sterol is steamed to remove n-hexane at 37 ℃ and-0.09 MPa to obtain 2.3 g of enriched 4,4' -dimethyl sterol;
(4) adding 2.3 g of the enriched 4,4 '-dimethyl sterol into 23mL of ethanol, heating to 60 ℃ for dissolving, cooling the solution to 25 ℃ for crystallization, growing crystals for 8 hours, and separating to obtain 4,4' -dimethyl sterol crystals, wherein the yield is 46.9%.
FIG. 1 is a normal phase high performance liquid chromatogram (HPLC-FID) of 4-methyl free sterol (stigmasterol) and 4,4' -dimethyl sterol (lupeol) standards.
FIG. 2 is a high performance liquid chromatogram of 4,4 '-dimethyl sterol obtained from Shea butter after extraction, wherein the chromatographic peak with retention time of 4.541min is 4,4' -dimethyl sterol, and the purity is 75.2% by peak area normalization.
Note: the raw materials used in the invention are purchased from Shea butter manufacturers, and have two types of refining and non-refining, and the commodity numbers are 7275849 (refined Shea butter, Kyozhou Kaimes chemical Co., Ltd.) and 170927 (Shea butter, Wuxi Okang food Co., Ltd.).
Example 2
(1) Taking 30 g of shea butter, filling the shea butter into a flask, saponifying, adding 200mL of 1mol/L potassium hydroxide ethanol solution, refluxing and saponifying at 105 ℃ for 1h, and collecting saponified oily liquid;
(2) adding 250mL of petroleum ether into the saponified oily liquid, layering, discharging the lower layer of liquid, taking the organic layer of the upper layer of feed liquid, washing twice with 250mL of warm water at 55 ℃, and separating liquid to obtain feed liquid containing 4,4' -dimethyl sterol;
(3) evaporating feed liquid containing 4,4 '-dimethyl sterol at 37 ℃ and-0.09 MPa to remove petroleum ether, and obtaining 3.2 g of enriched 4,4' -dimethyl sterol;
(4) adding 2.3 g of the enriched 4,4 '-dimethyl sterol into 50mL of acetone, heating to 65 ℃ for dissolving, cooling the solution to 30 ℃ for crystallization, growing crystals for 10 hours, and separating to obtain 4,4' -dimethyl sterol crystals, wherein the yield is 67.2%. FIG. 3 is a high performance liquid chromatogram of the prepared 4,4 '-dimethylsterol, wherein the chromatographic peak with retention time of 4.541min is 4,4' -dimethylsterol, and the purity is 89.1% by peak area normalization.
Example 3
(1) Taking 30 g of shea butter, filling the shea butter into a flask, saponifying, adding 200mL of 1mol/L potassium hydroxide ethanol solution, refluxing and saponifying at 105 ℃ for 1h, and collecting saponified oily liquid;
(2) adding 250mL of normal hexane into the saponified oily liquid, layering, discharging the lower layer of liquid, taking the organic layer of the upper layer of feed liquid, washing twice with 300mL of warm water at 85 ℃, and separating liquid to obtain feed liquid containing 4,4' -dimethyl sterol;
(3) evaporating feed liquid containing 4,4 '-dimethyl sterol at 37 ℃ and-0.09 MPa to remove n-hexane to obtain 4.2 g of enriched 4,4' -dimethyl sterol;
(4) adding 4.2 g of the enriched 4,4 '-dimethyl sterol into 100mL of mixed solution (1:2, v/v) of ethanol and isopropanol, heating to 75 ℃ for dissolution, cooling the solution to 25 ℃ for crystallization, growing crystals for 12h, and separating to obtain 4,4' -dimethyl sterol crystals, wherein the yield is 62.3%. FIG. 4 is a high performance liquid chromatogram of 4,4 '-dimethyl sterol obtained after extraction, in which the chromatographic peak with retention time of 4.541min is 4,4' -dimethyl sterol, and the purity is 95.6% by peak area normalization method.
FIG. 5 is a reverse phase high performance liquid chromatogram (RE-HPLC-ELSD) of the pure 4,4' -dimethylsterol obtained in this example; wherein, the figure shows firstly lupeol, secondly butyryl cetanol and thirdly resinol. As can be seen in FIG. 5, this figure illustrates that the composition of the pure 4,4' -dimethylsterol end product comprises lupeol, butyrospermol, and balsamic alcohol.
Example 4
(1) Taking 30 g of shea butter, filling the shea butter into a flask, saponifying, adding 200mL of 1mol/L potassium hydroxide ethanol solution, refluxing and saponifying at 105 ℃ for 1h, and collecting saponified oily liquid;
(2) adding 300mL of diethyl ether into the saponified oily liquid, layering, discharging the lower layer of liquid, taking the organic layer of the upper layer of feed liquid, washing twice with 350mL of warm water at 65 ℃, and separating liquid to obtain feed liquid containing 4,4' -dimethyl sterol;
(3) evaporating feed liquid containing 4,4 '-dimethyl sterol at 37 ℃ and-0.09 MPa to remove ether, and obtaining 2.6 g of enriched 4,4' -dimethyl sterol;
(4) adding 2.6 g of enriched 4,4 '-dimethyl sterol into 78mL of butanone at 75 ℃ for dissolving, cooling the solution to 30 ℃ for crystallization, growing crystals for 12 hours, separating to obtain 4,4' -dimethyl sterol crystals, and determining the purity to be 90.6% and the yield to be 52.9%.
Example 5
(1) Taking 30 g of shea butter, filling the shea butter into a flask, saponifying, adding 200mL of 1mol/L potassium hydroxide ethanol solution, refluxing and saponifying at 105 ℃ for 1h, and collecting saponified oily liquid;
(2) adding 250mL of dichloromethane into the saponified oily liquid, layering, discharging the lower layer of liquid, taking the organic layer of the upper layer of feed liquid, washing twice with 250mL of warm water at 55 ℃, and separating liquid to obtain feed liquid containing 4,4' -dimethyl sterol;
(3) evaporating feed liquid containing 4,4 '-dimethyl sterol at 37 ℃ and-0.09 MPa to remove dichloromethane, and obtaining 3.5 g of enriched 4,4' -dimethyl sterol;
(4) adding 3.5 g of enriched 4,4 '-dimethyl sterol into 50mL of mixed solution (1:1, v/v) of acetone and butanone at 75 ℃ for dissolving, cooling the solution to 35 ℃ for crystallization, growing crystals for 14h, and separating to obtain 4,4' -dimethyl sterol crystals with the purity of 95.3% and the yield of 34.9%.
Example 6
(1) Taking 30 g of shea butter, filling the shea butter into a flask, saponifying, adding 200mL of 1mol/L potassium hydroxide ethanol solution, refluxing and saponifying at 105 ℃ for 1h, and collecting saponified oily liquid;
(2) adding 250mL of normal hexane into the saponified oily liquid, layering, discharging the lower layer of liquid, taking the organic layer of the upper layer of feed liquid, washing twice with 300mL of warm water at 75 ℃, and separating liquid to obtain feed liquid containing 4,4' -dimethyl sterol;
(3) evaporating feed liquid containing 4,4 '-dimethyl sterol at 37 ℃ and-0.09 MPa to remove n-hexane to obtain 4.6 g of enriched 4,4' -dimethyl sterol;
(4) adding 4.6 g of enriched 4,4 '-dimethyl sterol into 100mL of mixed solution (2:1, v/v) of isopropanol and n-butanol at 75 ℃ for dissolving, cooling the solution to 45 ℃ for crystallization, growing crystals for 16h, separating to obtain 4,4' -dimethyl sterol crystals, wherein the determination purity is 92.3%, and the yield is 45.4%.
Example 7
(1) Taking 30 g of shea butter, filling the shea butter into a flask, saponifying, adding 200mL of 1mol/L potassium hydroxide ethanol solution, refluxing and saponifying at 105 ℃ for 1h, and collecting saponified oily liquid;
(2) adding 250mL of normal hexane into the saponified oily liquid, layering, discharging the lower layer of liquid, taking the organic layer of the upper layer of feed liquid, washing twice with 300mL of warm water at 85 ℃, and separating liquid to obtain feed liquid containing 4,4' -dimethyl sterol;
(3) evaporating feed liquid containing 4,4 '-dimethyl sterol at 37 ℃ and-0.09 MPa to remove n-hexane to obtain 4.2 g of enriched 4,4' -dimethyl sterol;
(4) 4.6 g of the enriched 4,4 '-dimethyl sterol is added into 100mL of mixed solution (1:2, v/v) of ethanol and isopropanol to be dissolved at 75 ℃, then the solution is cooled to 25 ℃ to be crystallized, crystallized for 12 hours, and separated to obtain 4,4' -dimethyl sterol crystals with the purity of 93.6 percent and the yield of 61.1 percent.
Example 8
(1) Taking 30 g of shea butter, filling the shea butter into a flask, saponifying, adding 200mL of 1mol/L potassium hydroxide ethanol solution, refluxing and saponifying at 105 ℃ for 1h, and collecting saponified oily liquid;
(2) adding 150mL of petroleum ether into the saponified oily liquid, layering, discharging the lower layer of liquid, taking the organic layer of the upper layer of feed liquid, washing twice with 200mL of warm water at 75 ℃, and separating liquid to obtain feed liquid containing 4,4' -dimethyl sterol;
(3) evaporating feed liquid containing 4,4 '-dimethyl sterol at 37 ℃ and-0.09 MPa to remove petroleum ether to obtain 3.1 g of enriched 4,4' -dimethyl sterol;
(4) adding 3.1 g of enriched 4,4 '-dimethyl sterol into 80mL of mixed solution (1:1, v/v) of ethanol and isobutanol at 65 ℃ for dissolving, cooling the solution to 25 ℃ for crystallization, growing crystals for 12h, and separating to obtain 4,4' -dimethyl sterol crystals, wherein the purity is 94.7% and the yield is 53.7%.
Example 9
(1) Taking 30 g of shea butter, filling the shea butter into a flask, saponifying, adding 200mL of 1mol/L potassium hydroxide ethanol solution, refluxing and saponifying at 105 ℃ for 1h, and collecting saponified oily liquid;
(2) adding 150mL of normal hexane into the saponified oily liquid, layering, discharging the lower layer of liquid, taking the organic layer of the upper layer of feed liquid, washing twice with 600mL of warm water at 80 ℃, and separating liquid to obtain feed liquid containing 4,4' -dimethyl sterol;
(3) evaporating feed liquid containing 4,4 '-dimethyl sterol at 37 ℃ and-0.09 MPa to remove n-hexane to obtain 4.3 g of enriched 4,4' -dimethyl sterol;
(4) 4.3 g of the enriched 4,4 '-dimethyl sterol is added into 100mL of mixed solution (2:1, v/v) of isopropanol and n-butanol at the temperature of 60 ℃ for dissolution, the solution is cooled to 25 ℃ for crystallization, crystal growth is carried out for 12 hours, 4' -dimethyl sterol crystals are obtained by separation, the purity is 81.6 percent, and the yield is 63.3 percent.
Example 10
(1) Taking 30 g of unrefined shea butter, filling into a flask, saponifying, adding 200mL of 1mol/L potassium hydroxide ethanol solution, performing reflux saponification at 105 ℃ for 1h, and collecting saponified oily liquid;
(2) adding 200mL of n-hexane into the saponified oily liquid, layering, discharging the lower layer of liquid, taking the organic layer of the upper layer of feed liquid, washing twice with 800mL of warm water at 75 ℃, and separating liquid to obtain feed liquid containing 4,4' -dimethyl sterol;
(3) evaporating feed liquid containing 4,4 '-dimethyl sterol at 37 ℃ and-0.09 MPa to remove n-hexane to obtain 3.5 g of enriched 4,4' -dimethyl sterol;
(4) adding 3.5 g of the enriched 4,4 '-dimethyl sterol into 80mL of mixed solution (1:1, v/v) of ethanol and isopropanol at 85 ℃ for dissolving, cooling the solution to 35 ℃ for crystallization, growing crystals for 12 hours, and separating to obtain 4,4' -dimethyl sterol crystals, wherein the purity is 90.3% and the yield is 42.8%.
Thus, example 3 is more effective, with less solvent consumption, shorter time, higher purity and higher recovery. It is worth mentioning that, in the inventive process of the present invention, compared with the patent CN1470519A, the method for preparing the alisma total sterol extract by carbon dioxide supercritical fluid extraction has the advantages of simple process flow, low requirement on equipment, and suitability for industrial production. Compared with the patent CN103080124A, the method has the advantages of low energy consumption and greatly reduced production cost by using mixed hydrolysate and low-polarity organic solvent to extract sterol. Compared with the preparation process of extracting phytosterol from rice bran crude oil in the patent CN102898491, the obtained 4,4' -dimethyl sterol has high utilization rate and purity, and can be directly used in the fields of medicine, chemical industry and the like.
The method takes the shea butter as a raw material, and the concomitant components in the shea butter mainly comprise 4,4 '-dimethyl sterol, so that the method is favorable for separating and preparing the high-purity 4,4' -dimethyl sterol. The inventor replaces shea butter with rice oil, and the experimental result shows that the final product has more impurities (tocopherol, tocotrienol, polyphenol and the like), and the purity of the obtained 4,4' -dimethyl sterol is low. In addition, the shea butter has high saturated fat content and is solid at normal temperature, and because the melting point is higher, the residual saturated fatty acid salt in the saponification process is easier to remove in the subsequent physical separation process.
According to the invention, the potassium hydroxide ethanol solution is used for saponification treatment, the saponification temperature is 105 ℃, the saponification time is 1h, triglyceride and 4,4' -dimethyl sterol ester are respectively converted into free fatty acid and free 4,4' -dimethyl sterol, the problem that the 4,4' -dimethyl sterol ester is difficult to separate due to the fact that the physical properties are too close to triglyceride is avoided, the polarity difference of the triglyceride and the free 4,4' -dimethyl sterol ester is enhanced, and the separation and purification of the 4,4' -dimethyl sterol are facilitated.
According to the invention, a certain amount of solvent is added into the saponified oily liquid to extract 4,4 '-dimethyl sterol, and the inventor finds that excessive solvent is easy to cause waste and is not beneficial to subsequent desolventizing treatment, the energy consumption is increased in the solvent evaporation process, and the excessive solvent is easy to emulsify and coagulate in the water adding washing process, so that the 4,4' -dimethyl sterol cannot be effectively separated, and the ratio of the solvent to the shea butter raw material is preferably 4-10: 1, in mL/g.
Adding a solvent into the enriched 4,4 '-dimethyl sterol, heating to 60-85 ℃ for dissolving, and cooling and crystallizing for 8-16 h at 25-45 ℃ to obtain a pure 4,4' -dimethyl sterol product. The inventor finds that the dissolution temperature is too low, so that the enriched solvent is insufficient, and a small amount of solid still remains in the system; if the temperature of the solvent is too high, the solvent is easy to volatilize, and the subsequent crystallization separation is not facilitated, so that the preferable dissolving temperature is 60-85 ℃.
In summary, the invention selects the shea butter rich in 4,4' -dimethyl sterol as the raw material, and combines a chemical method and a physical method, wherein the chemical saponification reaction converts triglyceride and 4,4' -dimethyl sterol ester into free fatty acid and free 4,4' -dimethyl sterol respectively, so as to strengthen the polarity difference between the triglyceride and the 4,4' -dimethyl sterol, and avoid the technical difficulties of similar properties such as boiling point and solubility when directly separating the triglyceride and the 4,4' -dimethyl sterol ester from the shea butter. In addition, saponification is beneficial to the subsequent physical crystallization, separation and purification of 4,4 '-dimethyl sterol, and the 4,4' -dimethyl sterol crystal obtained by separation has the advantages of yield of 62.3%, purity of 95.6%, and high product yield and purity.
The method has high extraction efficiency, and is suitable for refined shea butter and shea butter with wide adaptability to the raw material shea butter, poor quality or longer storage time. In particular, the method can recycle the used solvent, fully utilizes resources, reduces production cost, is suitable for industrial production, and has great application potential.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (1)
1. A method for extracting and preparing 4,4' -dimethyl sterol from shea butter is characterized in that: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
taking shea butter as a raw material, adding a potassium hydroxide ethanol solution for saponification, and collecting saponified oily liquid, wherein the weight ratio of the raw material to the saponified oily liquid is as follows: measured by mL, shea butter raw material: the potassium hydroxide ethanol solution was 3: 20; the concentration of the potassium hydroxide ethanol solution is 1mol/L, the saponification temperature is 105 ℃, and the saponification time is 1 h;
adding n-hexane into the saponified oily liquid, layering, taking out an organic layer, adding 85 ℃ water, washing twice, and separating to obtain a feed liquid containing 4,4' -dimethyl sterol, wherein the weight ratio of the organic layer to the solvent is mL: g, n-hexane: the shea butter raw materials are 25: 3, the volume ratio of water to n-hexane is 6: 5;
evaporating feed liquid containing 4,4 '-dimethyl sterol at 37 ℃ and under the pressure of-0.09 MPa, and removing a solvent to obtain an enrichment substance of 4,4' -dimethyl sterol;
adding a solvent into the enriched 4,4 '-dimethyl sterol, heating to 75 ℃ for dissolving, cooling and crystallizing to obtain a pure 4,4' -dimethyl sterol product, wherein the cooling and crystallizing temperature is 25 ℃, the crystal growing time is 12 hours, the solvent is a mixed solution of ethanol and isopropanol according to a volume ratio of 1:2, and the weight ratio of the ethanol to the isopropanol is g: mL, enrichment of 4,4' -dimethyl sterol: the solvent is 4.2: 100, respectively;
the 4,4' -dimethyl sterol comprises lupeol, butyryl cetanol and balsamic alcohol.
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