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Method for separating and extracting squalene in mixed tocopherols

An extraction method, the technology of squalene, applied in the field of separation and extraction of squalene, can solve the problems of unobvious extraction effect, difficult regeneration of adsorbent, small separation scale, etc., so as to improve the adsorption and separation effect and improve the scale utilization efficiency , Guarantee the effect of purity and recovery rate

Active Publication Date: 2013-09-11
NINGBO DAHONGYING BIO ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The saponification separation method has an obvious effect of removing fatty acids and glycerides at one time, and significantly increases the content of squalene, but the operation process is complicated, and a large amount of lower alcohol is required in the reaction process, and it is carried out under alkaline conditions, which is very destructive to the target product;
[0006] Molecular distillation is especially suitable for laboratory separation and is also easy to industrialize, but the cost is high, and the content of the target product in the raw material is low, the extraction effect is not obvious, and pretreatment is required;
[0007] The supercritical extraction method is direct extraction, which is environmentally friendly and non-polluting, but the components in the raw materials have high solubility in supercritical carbon dioxide, so the separation efficiency is not high, and the investment and operating costs are relatively large;
[0008] The adsorption separation method has good separation effect and high product purity, which is suitable for product purification, but the separation scale is small, the separation cost is high, some eluents are easy to pollute the product, and the regeneration of the adsorbent is difficult;
[0009] The solvent extraction process and equipment are simple, and the operating cost is low, but the polarity of squalene in natural products is very small, the enrichment effect of the solvent extraction method is obvious, and the amount of solvent used is large (6-10 times the volume of the raw material), resulting in difficulty in recovery and environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Take 70g of 100-200 mesh coarse-pore silica gel, add a small amount of n-hexane, fill it into the chromatographic column, elute the compacted silica gel with n-hexane 3 times the volume of the chromatographic column, and mix 5g of 50% mixed tocopherol and n-hexane by 2 : 1 (m / m) to dissolve and load the sample. After the sample is loaded, it is first eluted with 3 times the volume of n-hexane, and then eluted with a mixed solvent of n-hexane and ethyl acetate that is 3 times the volume of the chromatography column. The volume ratio of ethyl acetate is 15:1. The eluate was collected in sections and concentrated to obtain the squalene product with a content of 92.56% and a yield of 87.7%. The silica gel column was washed and regenerated with 2 times the volume of methanol.

Embodiment 2

[0035] Take 70g of 100-200 mesh coarse-pore silica gel, add a small amount of cyclohexane, fill it into the chromatographic column, elute the compacted silica gel with cyclohexane 3 times the volume of the chromatographic column, and mix 6.5g of 50% mixed tocopherol with cyclohexane Dissolve hexane at a ratio of 2:1 (m / m), add 5g of silica gel and stir evenly, then add to the top of the silica gel column, first elute with 3 times the volume of cyclohexane, then use 3 times the volume of the chromatography column with cyclohexane and A mixed solvent of ethyl acetate was used for elution, and the volume ratio of cyclohexane to ethyl acetate was 10:1. The eluate was collected in sections and concentrated to obtain the squalene product with a content of 90.28% and a yield of 84.6%. The silica gel column was washed and regenerated with 2 times the volume of ethyl acetate.

Embodiment 3

[0037]Take 100g of 100-200 mesh coarse-pore silica gel, add a small amount of petroleum ether, fill it into the chromatography column, elute the compacted silica gel with petroleum ether 3 times the volume of the chromatography column, and mix 7g of 30% mixed tocopherol and petroleum ether by 2 : 1 (m / m) to dissolve and load the sample. After the sample is loaded, it is eluted with 3 times the volume of petroleum ether, and then eluted with a mixed solvent of petroleum ether and ethyl acetate that is 3 times the volume of the column. Petroleum ether and ethyl acetate The volume ratio of ethyl acetate is 12:1. The eluate was collected in sections and concentrated to obtain the squalene product with a content of 90.8% and a yield of 86.6%. The silica gel column was washed and regenerated with 2 times the volume of methanol.

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Abstract

The invention provides a method for separating and extracting squalene in mixed tocopherols. The method comprises steps of: filling silochrom with the meshes of 100-200 into a chromatographic column, adopting an elution solvent to elute and compact the silochrom, then feeding the tocopherols into the chromatographic column according to a proper ratio, and separating the squalene from natural vitamin E through utilizing column chromatography. By adopting the separating and extracting method, the technological process is simple, the purity and recovery rate of the squalene can be improved to the maximum extent through utilizing a gradient elution method, silicagel columns can be well regenerated through utilizing strong polar solvents such as methyl alcohol and the like, and the method has the advantages of large solvent usage, easiness in recycling, small consumption and small environmental pollution.

Description

technical field [0001] The invention relates to a method for separating and extracting squalene, in particular to a method for separating and extracting squalene from natural vitamin E. Background technique [0002] Vitamin E (Vitamin E), also known as tocopherol, refers to a class of substances with α-tocopherol biological activity, is a fat-soluble vitamin, easily soluble in organic solvents such as fat and ethanol, insoluble in water, and is , Acid stable, unstable to alkali, sensitive to oxygen, insensitive to heat, is one of the most important antioxidants. The most important physiological function of tocopherol to the human body is to promote reproduction. It can promote the secretion of sex hormones, protect T lymphocytes, protect red blood cells, resist free radical oxidation, inhibit platelet aggregation, and reduce the risk of myocardial infarction and cerebral infarction. It also has a good improvement effect on burns, frostbite, capillary bleeding, menopausal s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C11/21C07C7/12
Inventor 张源仁王嘉磊肖翔章小平张海良杨伟潇李家培
Owner NINGBO DAHONGYING BIO ENG
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