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Separation method of tocopherol homologous compounds

A separation method and technology of tocopherol, which is applied in the field of lipid processing, can solve the problems of large preparation volume and strong load capacity, and achieve the effects of less sample loss, convenient operation and simple process

Active Publication Date: 2016-07-20
COFCO GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] (3) Large amount of preparation: Since no solid-phase filler is used, there is no void volume of the filler in the column, and the space in the column is all effective space, so the loading capacity is strong and the preparation amount is large
[0018] There is no report in the field of separation of mixtures of tocopherol homologues using HSCCC technology

Method used

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  • Separation method of tocopherol homologous compounds
  • Separation method of tocopherol homologous compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] The tocopherol mixture used in this example is mixed tocopherol. As determined by HPLC method, the total content of α-tocopherol, (β+γ)-tocopherol and δ-tocopherol is 96.5wt%. Among them, α-tocopherol The content of phenol was 22.9 wt%; the content of (β+γ)-tocopherol was 35.8 wt%; the content of δ-tocopherol was 37.8 wt%.

[0081] (1) According to the ratio of n-heptane: ethanol: water = 5:5:1 (v / v / v), the above three solvents are added to the separatory funnel, shaken 2-3 times and fully mixed, then stand to separate phase, to obtain a two-phase mixed solution; use a clean reagent bottle to collect the upper phase solvent and the lower phase solvent in the two-phase mixed solution, put them into an ultrasonic oscillator for degassing treatment, stand still after degassing for 25 minutes, and wait for The solvent was returned to room temperature.

[0082] (2) Take 1.052g of tocopherol mixture and dissolve it in 20ml of the upper phase solvent obtained in step (1) as t...

Embodiment 2

[0087] The tocopherol mixture used in this example is mixed tocopherol, and the total content of α-tocopherol, (β+γ)-tocopherol and δ-tocopherol is 92.1wt% as determined by HPLC method, wherein α-tocopherol The content of phenol was 21.8 wt %; the content of (β+γ)-tocopherol was 33.4 wt %; the content of δ-tocopherol was 36.9 wt %.

[0088] (1) According to the ratio of n-hexane: methanol: water = 30:30:0.5 (v / v / v), add the above three solvents to the separatory funnel, shake for 2-3 times and mix thoroughly, then let stand for phase separation , to obtain a two-phase mixture; use a clean reagent bottle to collect the upper phase solvent and the lower phase solvent in the two-phase mixture, put them into an ultrasonic oscillator for degassing treatment, stand still after degassing for 25 minutes, and wait for the solvent Return to room temperature.

[0089] (2) Take 1.034g of tocopherol mixture and dissolve it in 20ml of the upper phase solvent obtained in step (1) as the sam...

Embodiment 3

[0094] The tocopherol mixture used in this example is mixed tocopherol, and the total content of α-tocopherol, (β+γ)-tocopherol and δ-tocopherol is 52.8wt% as determined by HPLC method, wherein α-tocopherol The content of phenol was 7.8 wt%; the content of (β+γ)-tocopherol was 30.4 wt%; the content of δ-tocopherol was 14.6 wt%.

[0095] (1) According to the ratio of n-heptane:methanol:water=25:25:1 (v / v / v), the above three solvents are added to the separatory funnel, shaken 2-3 times and fully mixed, then stand to separate phase, to obtain a two-phase mixed solution; use a clean reagent bottle to collect the upper phase solvent and the lower phase solvent in the two-phase mixed solution, put them into an ultrasonic oscillator for degassing treatment, stand still after degassing for 25 minutes, and wait for The solvent was returned to room temperature.

[0096] (2) Take 1.003g of tocopherol mixture and dissolve it in 20ml of the upper phase solvent obtained in step (1) as the ...

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Abstract

The invention provides a separation method of tocopherol homologous compounds. The method comprises the steps of: (1) mixing well one or more polar solvents with one or more non-polar solvents, and standing for phase separation to obtain an upper phase solvent and a lower phase solvent; (2) dissolving the tocopherol mixture in the upper phase solvent obtained in the step (1) as a sample to be separated; (3) using the upper phase solvent obtained in the step (1) as a stationary phase and the lower phase solvent obtained in the step (1) as a mobile phase, separating the sample to be separated in the step (2) by a high-speed countercurrent chromatography to obtain a mixed solution of tocopherol homologous compounds and the mobile phase, wherein the tocopherol homologous compounds comprise alpha-tocopherol, (beta + gamma)-tocopherol and delta-tocopherol; and (4) removing the mobile phase solvent in the mixed solution of tocopherol homologous compounds and the mobile phase obtained in the step (3), so as to obtain tocopherol homologous products.

Description

technical field [0001] The invention belongs to the field of lipid processing, in particular to a method for separating tocopherol homologues from natural mixed tocopherols. Background technique [0002] Natural vitamin E (scientific name tocopherol) is a mixture of 8 compounds including α-, β-, δ-, γ-tocopherol and tocotrienol corresponding to the above four tocopherols. Radical, anti-cancer, anti-cardiovascular disease, enhance immunity and anti-aging effects. [0003] The structural differences among the homologous compounds of tocopherol are very small. Such as figure 1 As shown, its basic structure consists of a 6-chromanol (6-hydroxylschroman) and a substituted saturated C at the 2' position of the chroman ring 16 composition of side chains. According to the position and quantity of the methyl group on the benzene ring of chromanol, it can be divided into four different compounds: α-, β-, γ-, and δ-tocopherol: Among them, α-tocopherol has 3 methyl groups (R 1 =-C...

Claims

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Application Information

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IPC IPC(8): C07D311/72
Inventor 赵抒娜林旭琦王满意林海龙车夏宁曹玉平蒋一鸣陈学兵周学晋
Owner COFCO GROUP
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