Method for extracting high-purity squalene by taking olive oil as raw material

A technology of squalene and olive oil, applied in the direction of adsorption purification/separation, distillation purification/separation, chemical change purification/separation, etc., can solve the problems of not obtaining higher purity squalene, etc., and achieve short heating time, The effect of cost reduction and stable quality

Active Publication Date: 2009-12-09
JIANGSU ZODIAC MARINE BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] But above-mentioned method all does not obtain squalene of higher purity

Method used

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  • Method for extracting high-purity squalene by taking olive oil as raw material
  • Method for extracting high-purity squalene by taking olive oil as raw material
  • Method for extracting high-purity squalene by taking olive oil as raw material

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Apply saponification acidification, secondary molecular distillation and silica gel column chromatography to separate and purify squalene in olive oil, comprising the following steps:

[0026] 1) Preparation of olive oil unsaponifiables: Take 30g of olive oil, 6g of KOH, and 60mL of 95% ethanol, put them into a three-necked flask, use nitrogen as a protective gas to react under constant stirring, and reflux in a water bath at 100°C for 10h. After stopping the reaction, quickly add 200mL of distilled water, extract the unsaponifiable matter with 250mL of petroleum ether five times, add HCL and 5% NaCl aqueous solution to wash the ether phase, and finally wash with water until the lotion is neutral. Add an appropriate amount of anhydrous Na 2 SO 4 Absorb the residual moisture in the ether phase, and remove the solvent by rotary evaporation at 60°C to obtain the olive oil unsaponifiable matter, which can be detected by liquid chromatography to obtain a purity of 43.71% of...

Embodiment 2

[0030] Basic technology is with embodiment 1, and concrete operation parameter is as follows:

[0031] 1) Preparation of olive oil unsaponifiable matter: Take 30g of olive oil, 6g of KOH, and 60mL of 95% ethanol, add them into a three-necked flask, use nitrogen as a protective gas to react under constant stirring, and reflux in a water bath at 60°C for 1h. After stopping the reaction, quickly add 200mL of distilled water, extract the unsaponifiable matter with 250mL of petroleum ether five times, add HCL and 5% NaCl aqueous solution to wash the ether phase, and finally wash with water until the lotion is neutral. Add an appropriate amount of anhydrous Na 2 SO 4 Absorb the residual moisture in the ether phase, and remove the solvent by rotary evaporation at 60°C to obtain the unsaponifiable product of olive oil, in which the purity of squalene is 47.33%.

[0032]2) Separation of crude squalene by two-stage molecular distillation: the unsaponifiable matter of olive oil was sen...

Embodiment 3

[0035] Basic technology is with embodiment 1, and concrete operation parameter is as follows:

[0036] 1) Preparation of olive oil unsaponifiable matter: Take 30g of olive oil, 6g of KOH, and 60mL of 95% ethanol, add them into a three-necked flask, use nitrogen as a protective gas, react under constant stirring, and reflux in a water bath at 120°C for 5h. After stopping the reaction, quickly add 200mL of distilled water, extract the unsaponifiable matter with 250mL of petroleum ether five times, add HCL and 5% NaCl aqueous solution to wash the ether phase, and finally wash with water until the lotion is neutral. Add an appropriate amount of anhydrous Na 2 SO 4 Absorb the residual moisture in the ether phase, and remove the solvent by rotary evaporation at 60°C to obtain the olive oil unsaponifiable product, in which the purity of squalene is 44.60%.

[0037] 2) Separation of crude squalene by two-stage molecular distillation: send olive oil unsaponifiables into a primary mol...

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Abstract

The invention relates to a method for extracting high-purity squalene by taking olive oil as a raw material. A technological route formed by adopting a secondary molecular distillation and silica gel column chromatography is as follows: an olive oil unsaponifiable substance is taken, squalene is separated and purified by using two stages of molecular distillation, primary molecular distillation is carried out under the conditions of the evaporation surface temperature of 100 to 200 DEG C, the systemic pressure of 0.001 to 0.01mbar and the scraping film rotor speed of 150 to 300rpm, and secondary molecular distillation is carried out to the obtained distillate; the secondary molecular distillation is carried out under the conditions of the evaporation surface temperature of 150 to 300 DEG C, the systemic pressure of 0.001 to 0.01mbar and the scraping film rotor speed of 200 to 350rpm, and the obtained distillate is a squalene crude product; ethyl acetate-normal hexane with different concentrations is used as a mobile phase to carry out gradient elution, the obtained eluent is collected according to time and a solvent is evaporated, the same fractions are merged through chromatographic detection, and the high-purity squalene can be obtained, wherein the content of the raw material olive oil of the squalene is enhanced from 3.6% to about 98%; and especially, by considering the requirement of industrialized production to select an extraction condition especially, the large-scale production of the squalene taking the olive oil as the raw material can be realized.

Description

technical field [0001] The invention relates to the extraction technology of high-purity squalene, in particular to a method for extracting high-purity squalene from olive oil. Background technique [0002] Olive oil is recognized as a "green food" in edible oils, with a stable source and a huge output. The high level of fat contained in olive oil retains almost all the nutrients and has extremely high nutritional value for the human body. Studies have shown that the content of squalene in olive oil is relatively high in vegetable oils. Years of studies have confirmed that squalene is a natural antioxidant with various physiological functions and is an irreplaceable important substance in the human body. Most of the squalene ingredients in cosmetics and health products currently used by humans come from shark liver oil. Human activities have led to the depletion of marine fishery resources, so the process of extracting squalene from shark liver oil will gradually be restr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C11/21C07C7/04C07C7/12C07C7/148
CPCC07C7/04C07C7/12
Inventor 徐世民戴宇航丁辉张艳华
Owner JIANGSU ZODIAC MARINE BIOTECH
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