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Squalene extracting method

A technology of squalene and raw materials, applied in chemical instruments and methods, purification/separation of hydrocarbons, steroids, etc., can solve the problems of large solvent consumption, high material consumption and energy consumption, and low recovery rate of squalene, and achieve The effect of less organic solvent

Active Publication Date: 2015-11-04
COFCO NUTRITION & HEALTH RES INST +2
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The purpose of the present invention is to overcome the problems of high material consumption and energy consumption, low squalene recovery rate and low feasibility of large-scale production in the existing method for extracting squalene, and provide a method for extracting squalene
[0011] The inventors of the present invention found that during the extraction process, the squalene in the raw material is enriched first, and then chromatographic chromatography is performed, thereby solving the problems of large solvent consumption, high material consumption and energy consumption caused by direct chromatographic chromatography , so as to make the extraction process more economical and effective under the premise of ensuring a relatively high extraction purity of squalene, and improve the feasibility of large-scale production of squalene extraction technology

Method used

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Examples

Experimental program
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Effect test

Embodiment approach

[0059] In the present invention, the first chromatographic separation can adopt the method used in the patent application with publication number CN101475557A. According to one embodiment of the present invention, the first chromatographic separation process includes: taking the fraction rich in vitamin E and squalene obtained by the first molecular distillation, dissolving it in absolute ethanol and loading the sample, and the chromatographic filler can be an anion exchange resin , the mobile phase can be absolute ethanol. Wash with mobile phase after sample loading, collect unadsorbed substances, and obtain squalene-rich raw materials. Then flush into the chromatographic column acid gas, such as carbon dioxide gas, etc. for desorption, and then wash with the mobile phase, and the collected desorption phase is the liquid phase rich in vitamin E, and the liquid phase rich in vitamin E is concentrated. And then refined, you can get high-purity vitamin E.

[0060] In the prese...

preparation example

[0068] Take 1000g of rapeseed oil deodorization distillate (the composition and related parameters are shown in Table 1, and the rest are impurities), add 35g of concentrated sulfuric acid and 300g of methanol to carry out esterification reaction at 70°C, and the esterification reaction product is washed with water and evaporated Dehydration to a moisture content below 0.4% by weight, and then adding 40 g of sodium methoxide and 300 g of methanol to carry out transesterification reaction at a temperature of 70° C., and then the first crystallization separation of the transesterification reaction product. In the first crystallization separation step, the temperature is lowered to 15° C. at a cooling rate of 8° C. / h, and the crystal is maintained at this temperature for 10 hours, and then the first solid-liquid separation is carried out; the liquid obtained by the first solid-liquid separation is Carry out the second cooling, the cooling rate is 4°C / h, the temperature is lowered ...

Embodiment 1

[0077] Preheat 58 g of the squalene-rich raw material obtained in Preparation Example 1 to 55° C., and then dissolve it in a 55° C. mixture (first organic solvent) composed of 70 ml of anhydrous acetone and 45 ml of n-hexane. Then the resulting solution was cooled to 25°C for the first time at a speed of 4°C / h, maintained at this temperature for the first crystal growth for 10 hours, and filtered for the first time (solid-liquid separation), and the resulting filtrate was heated at 4°C The temperature was lowered to 5°C for the second time at a rate of 100°C, and the crystal was grown for the second time at this temperature for 10 hours, and then filtered for the second time, and the solid obtained from the second filtration was washed with absolute ethanol, recrystallized, dried, and collected. Phytosterols are obtained after refining.

[0078] The second liquid obtained after the second filtration is subjected to a second molecular distillation after thin film evaporation, w...

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Abstract

The invention relates to a squalene extracting method. The method comprises the steps of carrying out crystal separation on a squalene-enriched raw material to obtain a solid phase and a liquid phase; and sequentially carrying out evaporation, molecular distillation and chromatographic separation on the liquid phase, wherein the squalene-enriched raw material contains 5-30wt% of squalene and 10-40wt% of sterol. By using the method disclosed by the invention, squalene with higher purity can be obtained, meanwhile, vitamin E and plant sterol which have higher purity are obtained, the raw material is sufficiently utilized, and thus the material consumption and the energy consumption are reduced to the greater extent.

Description

technical field [0001] The invention relates to a method for extracting squalene. Background technique [0002] Squalene is a highly unsaturated hydrocarbon compound, its system name is 2,6,10,15,19,23-hexamethyl-2,6,10,14,18,22-tetradecano Hexaene, molecular formula C30H50, belongs to terpenoids. Squalene is widely distributed in animals and plants. Given its special chemical structure, squalene has many functions such as anti-oxidation, promoting skin health, promoting cardiovascular health, assisting in the prevention and treatment of tumors, and improving the human body's ability to withstand hypoxia. It is widely used in In the field of medicine and cosmetics, the application in the field of health care products has gradually expanded in recent years. [0003] The squalene on the market is mainly extracted from the liver oil of deep-sea sharks. At present, the number of deep-sea sharks is gradually decreasing, and some species are on the verge of extinction, which mak...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C11/21C07C7/00C07D311/72C07J9/00
Inventor 车夏宁赵抒娜王满意林海龙曹玉平蒋一鸣陈学兵周学晋
Owner COFCO NUTRITION & HEALTH RES INST
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