Method for separating and extracting sterol from wool fat

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 ...

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 CN 1958596A describes a column chromatography method to achieve product separation. First, lanolin is subjected to transesterification reaction, and then short-path distillation is carried out to obtain crude cholesterol, which is then loaded by wet method, and 90~120 mesh silica gel is used as chromatography 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%. During the experiment, the sodium soap obtained from the transesterification part was easily emulsified, making the soap Alcohol 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

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