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Method for extracting squalene in vegetable oil deodorizer distillate through two-stage column chromatography

A technology for deodorizing distillate and column chromatography, which is applied in the directions of steroids, adsorption purification/separation, chemical change purification/separation, etc. Extraction rate, short-term return, high separation efficiency

Inactive Publication Date: 2014-04-09
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Considering the current problems of cumbersome extraction steps, low efficiency and low pertinence of plant squalene, column chromatography is used to separate plant squalene by taking advantage of the high selectivity of column chromatography in the separation of natural products
But the composition of the deodorized distillate as raw material is complex, most of which are fatty acids and glycerides, and the content of squalene is generally less than 3%. Direct column chromatography not only has low separation efficiency and poor separation effect, but also has too much Impurities can clog the bed, rendering the process inoperable

Method used

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  • Method for extracting squalene in vegetable oil deodorizer distillate through two-stage column chromatography
  • Method for extracting squalene in vegetable oil deodorizer distillate through two-stage column chromatography
  • Method for extracting squalene in vegetable oil deodorizer distillate through two-stage column chromatography

Examples

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Effect test

Embodiment 1

[0042] This example will adopt the method that saponification pretreatment and secondary column chromatography combine to extract the squalene in soybean oil deodorization distillate, concrete implementation steps are:

[0043] 1. Separation of unsaponifiable matter: Take 108g of soybean oil deodorization distillate (squalene content 1.96%), add a small amount of TBHQ as a protective agent, add 1.5mol / L NaOH-methanol solution 320ml under stirring, 80℃ Saponify under reflux for 1 hour. After the reaction, add 300ml of distilled water, stir for 2 minutes, take it out and cool to room temperature. Petroleum ether was extracted three times, 500 mL each time, the petroleum ether layer was combined, and the petroleum ether layer was washed with 5% brine until neutral. After the petroleum ether layer was dehydrated, the solvent was removed by rotary evaporation at 60°C to obtain unsaponifiable matter, which was detected by GC-MS (attached figure 2 ), the content of squalene in unsa...

Embodiment 2

[0049] In this example, a combination of saponification pretreatment and secondary column chromatography will be used to extract squalene from rice bran oil deodorization distillate. The specific implementation steps are:

[0050] 1. Separation of unsaponifiable matter: Take 100g of rice bran oil deodorization distillate (0.86% squalene content), put the distillate into a three-neck round bottom flask, add a small amount of BHA as a protective agent while stirring, and then add 1.5mol / L KOH-ethanol solution (the amount added is 1.5 times the theoretical amount), reflux saponification at 80°C for 1.5h, after the reaction, add 300ml of distilled water, stir for 2 minutes, take it out and cool to room temperature. Extract with n-hexane three times, 500 mL each time, combine the n-hexane layers, and wash the n-hexane layers with 5% brine until neutral. After the n-hexane layer was dehydrated, the solvent was removed by rotary evaporation at 60°C, and the unsaponifiable matter wa...

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Abstract

The invention provides a method for extracting squalene in vegetable oil deodorizer distillate through two-stage column chromatography, which comprises the following processing steps: performing saponifying pretreatment to separate unsaponifiable matters, performing first-stage column chromatography to separate tocopherol and sterol, and performing second-stage column chromatography to purify squalene. Through the whole process, the squalene having a content of about 50% can be obtained, and meanwhile, the tocopherol having a content of 70% or above and the sterol having a content of 98% or above can be also obtained. Thus, the method provided by the invention overcomes the problem of low pertinence in the traditional squalene extraction process, achieves favorable selectivity of column chromatography and greatly increases the extraction efficiency. The process has the advantages of simple operation procedure, high separation efficiency, high squalene recovery rate, low investment and the like.

Description

technical field [0001] The invention relates to the field of squalene purification, in particular to a method for extracting squalene in vegetable oil deodorization distillate by secondary column chromatography. Background technique [0002] Squalene, the molecular formula is C 30 h 50 , molecular weight 410.7, chemical name is 2,6,10,15,19,23-hexamethyl-2,6,10,14,18,22-tetracosahexaene, which belongs to open-chain triterpenes. Squalene is a colorless or yellowish transparent oily liquid, easily soluble in n-hexane, ether, petroleum ether, acetone and carbon tetrachloride, slightly soluble in ethanol, insoluble in water. It is easy to oxidize, so an appropriate antioxidant should be added during preservation. [0003] Squalene has remarkable anti-oxidation and anti-radiation effects, and can strengthen immune regulation and enhance metabolism. In medicine, it is often used as an effective anti-tumor and anti-cancer drug, participates in the treatment of cardiovascula...

Claims

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Application Information

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IPC IPC(8): C07C11/21C07C7/148C07C7/12C07D311/72C07J9/00
Inventor 袁传勋琚裕杰金日生
Owner HEFEI UNIV OF TECH
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