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Method of extracting squalene from bottom sediment with natural vitamin E extracted

A technology of natural vitamins and squalene, applied in chemical instruments and methods, purification/separation of hydrocarbons, organic chemistry, etc., can solve problems such as inability to realize industrial production, single means of separation and purification, unreasonable sources of raw materials, etc., and achieve increase Added value, important economic effects, ease of handling

Active Publication Date: 2016-03-02
ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are related studies on extracting squalene from vegetable oils, but the current process route has many disadvantages. (1) The source of raw materials is unreasonable and the content is low. When extracting squalene, it does not involve the recovery of other substances in it. useful ingredients, so the production cost is too high, and it is not economically cost-effective; (2) The separation and purification method is single, and the separation efficiency is low and the content is not high without other high-efficiency separation processes; (3) Most of the current research is only in the experimental Preliminary explorations have been carried out on the laboratory scale, and the method cannot realize real industrial production

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0028] The preparation steps of embodiment 1 raw material unsaponifiable matter 1)

[0029] Get 500g leftover oil (the leftover oil used in this embodiment is the leftover oil in the current production of natural vitamin E process of Xinchang pharmaceutical factory, and its main composition is as follows: squalene 7.5%, natural vitamin E6.7%. Add 500mL of 20% KOH in methanol solution was filled with nitrogen at 70°C and saponified for 1 hour under the condition of reflux, then 500mL of distilled water at 60-70°C was added to terminate the reaction. Then 300mL of n-hexane was used to extract the unsaponifiable matter three times, and acidified with dilute sulfuric acid. Wash the n-hexane phase with 10% salt water, and finally wash to neutrality, and obtain 183g of unsaponifiable matter after vacuum removal of the solvent. Wherein squalene 33.3g (18.2%), natural vitamin E 31.8g (17.3%).

Embodiment 2

[0030] The preparation steps of embodiment 2 raw material unsaponifiable matter 1)

[0031] Get 500g leftover oil (the leftover oil used in this embodiment is the leftover oil in the current production of natural vitamin E process of Xinchang pharmaceutical factory, its main composition is as follows: squalene 7.5%, natural vitamin E6.7%. Add 1000mL of 20% KOH ethanol solution, fill with nitrogen at 70-80°C, saponify under reflux for 1 hour, then add 500mL of 70-80°C distilled water to terminate the reaction. Then use 300mL petroleum ether to extract the unsaponifiable matter three times, add Dilute sulfuric acid acidification, 10% salt water washes n-hexane phase, finally washes to neutrality, obtains unsaponifiable matter 168g after vacuum removal solvent.Wherein squalene 34.9g (20.8%), natural vitamin E31.8g (18.9%) ).

Embodiment 3

[0032] The preparation steps of embodiment 3 raw material unsaponifiable matter 1)

[0033] Get 1000g leftover oil (the leftover oil used in this embodiment is the leftover oil in the current production of natural vitamin E process of Xinchang pharmaceutical factory, and its main composition is as follows: squalene 7.5%, natural vitamin E6.7%. Add 1000mL methanol solution of 10% NaOH was filled with nitrogen at 70°C, saponified under reflux for 2h, then added 1000mL of distilled water at 70-80°C to terminate the reaction. Then extracted unsaponifiable matter with 500mL n-heptane three times, acidified with dilute hydrochloric acid , 10% salt water washing petroleum ether phase, final washing to neutrality, vacuum removal of solvent to obtain unsaponifiable 383g. Wherein squalene 67.8g (17.7%), natural vitamin E60.5g (15.8%).

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Abstract

The invention discloses a method of extracting squalene from bottom sediment with natural vitamin E extracted. The bottom sediment with the natural vitamin E extracted is used as the raw material to prepare high-content squalene through a saponification, rectification and silica gel column chromatography combined process. The method specifically comprises the steps that firstly, the bottom sediment is subjected to a saponification reaction, unsaponifiable matter obtained through extraction is subjected to separation in a secondary rectifying tower, distillate obtained through secondary rectification is used as the raw material and subjected to silica gel column chromatography separation, three organic solvents with different polarities are used for elution, and fractional collection is conducted to obtain a plant hydrocarbon component, a squalene component, a natural vitamin E component and a sterol component, wherein the squalene content of the squalene component is more than 95%. According to the method, the bottom sediment with the natural vitamin E extracted is used as the raw material for extraction of the squalene, the process is simple and convenient, separation efficiency is high, industrial production is easy, the obtained squalene content is high, crude natural vitamin E and sterol can also be obtained, and comprehensive utilization of effective ingredients in the bottom sediment is achieved.

Description

technical field [0001] The invention relates to a preparation of plant squalene, in particular to a method for preparing high-content squalene from scraps after extracting natural vitamin E. Background technique [0002] The chemical name of squalene is 2,6,10,15,19,23-hexamethyl-2,6,10,14,18,22-tetracosahexaene, as a lipid unsaponifiable, Widely distributed in most animals and plants, squalene has good biological activity and can be used as an effective drug for anti-tumor, anti-cancer, anti-infection and treatment of cardiovascular and cerebrovascular diseases. It is also widely used in beauty drugs and cosmetics. In addition, it can also be used as an antibacterial agent, lubricating oil, etc. [0003] At present, deep-sea shark liver oil is mostly used to extract squalene, but such a large-scale production of squalene will lead to ecological imbalance of deep-sea sharks. In recent years, Europe has begun to reduce the fishing of deep-sea species through strict quotas. T...

Claims

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Application Information

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IPC IPC(8): C07C11/21C07C7/04C07C7/00C07C7/12
Inventor 代志凯许新德邵斌
Owner ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
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