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Method for separating and extracting sterol from lanolin

A lanolin and sterol technology, applied in steroids, organic chemistry and other directions, can solve the problems of difficult control of solvent selection and extraction conditions, low product separation purity, expensive molecular distillation equipment, etc. The effect of high rate and low production cost

Inactive Publication Date: 2015-11-18
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method consumes less chemical auxiliary materials, but the molecular distillation equipment is expensive, and the solvent selection extraction condition parameters are difficult to control
Zhejiang University patent CN1958596A describes a column chromatography method to achieve product separation. First, transesterification is performed on lanolin, and then short-path distillation is carried out to obtain crude cholesterol. Then, samples are loaded by wet method, and 90~120 mesh silica gel is used as the chromatographic medium. , toluene and petroleum ether (ratio 70:30~95:5) were used as the mobile phase for elution to obtain cholesterol with a purity of 88%~90%. Separation is difficult; short-path distillation involves gradient temperature rise, and the final temperature is 200 ° C, which is dangerous to operate in industrialization; column chromatography steps, using continuous operation and isocratic elution, can complete the separation of sterols, but the purity is not high, and The operation needs to be carried out at a constant temperature of 30°C, which puts forward further requirements for the design of the chromatography column, and poses a greater challenge to the design of the column in industrialization
[0010] In order to solve the actual problems such as the emulsification of the reaction solution by sodium soap, the viscosity of the column chromatography sample, the constant temperature operation of the column chromatography, and the low purity of the product separation, this paper The patent relates to a method to solve the above problems and obtain high-purity sterols

Method used

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  • Method for separating and extracting sterol from lanolin
  • Method for separating and extracting sterol from lanolin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1. Weigh 25.000g of lanolin (containing about 11% cholesterol), put it into a 250mL three-necked bottle, add 150mL of ethanol, 2.679g of sodium hydroxide and 10mL of deionized water, heat to reflux temperature (80°C), and mechanically stir the reaction After 3-8 hours, the reaction was completed to obtain a brown-black mixed solution.

[0031] 2. Reduce the temperature of the reaction solution to 40~55°C, and adjust the pH value of the reaction solution to about 8.5~9, weigh 0.5 times the molar amount (relative to the amount of sodium hydroxide) of calcium chloride, and stir for 1~2 hours. The color of the reaction solution gradually becomes lighter, and a dark yellow mixture is obtained (a black residue will be obtained above 70°C, which is not conducive to the reaction).

[0032] 3. After the mixture was suction filtered, the residue was extracted with absolute ethanol (200mL×3) to obtain a khaki-colored calcium soap powder, and all the dark yellow filtrates were comb...

Embodiment 2

[0039] Operations were the same as steps 1-7 of Example 1 before the recrystallization step. Heat the obtained crude cholesterol to reflux and dissolve in ethyl acetate (8mL / g). When the solution is clear, add petroleum ether drop by drop. When adding petroleum ether just makes the solution cloudy, heat until clear and cool to crystal. Precipitate, finally obtain 2.07g cholesterol, purity 92.2%.

Embodiment 3

[0041] Operations were the same as steps 1-7 of Example 1 before the recrystallization step. Heat the obtained crude cholesterol to reflux and dissolve it in absolute ethanol (5mL / g). When the solution is clear, add water drop by drop. When adding petroleum ether just makes the solution cloudy, heat to clear and cool to crystals. , finally obtained 2.21g of cholesterol with a purity of 93.0%.

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Abstract

The invention discloses a method for separating and extracting sterol from wool fat. The method comprises the following step of: (1), carrying out saponification reaction on the wool fat in an alkali-alcohol solution; (2), carrying out saponification double decomposition on calcium chloride and the product obtained in the last step to obtain a calcium soap and wool alcohol; (3), filtering the obtained filtrate in vacuum, extracting under refluxing filter residue by utilizing low-level fatty alcohol, collecting filtrate and adding fatty acid to the filtrate to remove the residual calcium ion; (4), acidifying and bleaching filter cake to obtain the wool acid; and (5), carrying out recrystallization to obtain a refined product. The steps are carried out, so that the purity of obtained cholesterol is higher than 93% and the yield is more than 78%. The method disclosed by the invention has the advantages that the obtained product is high in purity and yield, excellent in color and crystal form and free of peculiar smell, the process flow is simple and easy to operate, and the solvent and the chromatography media in the process flow can be recycled without generating wastes, so that the process cost is low and the industrial production can be realized.

Description

technical field [0001] The invention belongs to the direction of biochemical separation and is used for separating and extracting sterols from lanolin. Specifically, it refers to a method for obtaining high-quality cholesterol, lanosterol and other sterols through processes such as saponification→metathesis→solvent selective extraction→column chromatography→recrystallization. Background technique [0002] As a well-known natural material, cholesterol has been widely used in the fields of cosmetics, materials, and biomedicine due to its various properties. ① From the perspective of biological factors, cholesterol has an affinity for cell membranes and can change the properties of cell membranes, which is of great significance for the application of polymers in drug sustained-release materials and tissue engineering. ②Important pharmaceutical intermediates, mainly used in the synthesis of vitamin D 3 , steroid drugs and related sex hormones. ③Cholesterol has multiple chiral ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J9/00
Inventor 谭天伟董森马凯琛周雅莉王斌刘广
Owner BEIJING UNIV OF CHEM TECH
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