Method for separating single tocopherol from mixed tocopherol

A technology for separating tocopherols, which is applied in the field of separating single tocopherols, and achieves the effects of high degree of production automation, simple process and high production efficiency

Inactive Publication Date: 2008-07-16
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the separation and purification of tocopherol homologs from SMBC has not been reported

Method used

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  • Method for separating single tocopherol from mixed tocopherol
  • Method for separating single tocopherol from mixed tocopherol
  • Method for separating single tocopherol from mixed tocopherol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Simulated moving bed system CSEP _ 916 (Norr, Germany), equipped with 8 chromatographic columns (ID2×10cm), 2 in each zone, the chromatographic columns are filled with silica gel, and the columns are packed by high-pressure wet method. The mobile phase was n-hexane / ethanol solution (99.5 / 0.5, v / v), and the temperature was 30°C. The purity of the mixed tocopherols used for feeding is 97.5%, which contains 22.8% of α-tocopherol, 2.8% of β-tocopherol, 34.7% of γ-tocopherol and 37.2% of δ-tocopherol. mg / ml feed solution.

[0034] a. Operating conditions

[0035] Injection liquid flow rate: U F =1ml / min

[0036] Eluent flow rate: U D =2.8ml / min

[0037] Raffinate flow rate: U R =2.0ml / min

[0038] Extraction flow rate: U E =1.8ml / min

[0039] Zone 1 velocity: U E =6.4ml / min

[0040] Switching time: t s =757s

[0041] b. Finished product analysis

[0042] The composition of raffinate and extract was analyzed by silica gel column. The purity and yield of δ-toco...

Embodiment 2

[0044] Simulated moving bed system CSEP_ 916 (Norr, Germany), equipped with 8 chromatographic columns (ID2×10cm), 2 in each zone, the chromatographic columns are filled with powdered activated carbon, and packed by high-pressure wet method. The mobile phase was n-hexane / methanol solution (99.5 / 0.5, v / v), and the temperature was 30°C. The purity of the mixed tocopherols used for feeding is 97.5%, which contains 22.8% of α-tocopherol, 2.8% of β-tocopherol, 34.7% of γ-tocopherol and 37.2% of δ-tocopherol. mg / ml feed solution.

[0045] a. Operating conditions

[0046] Injection liquid flow rate: U F =1ml / min

[0047] Eluent flow rate: U D =2.6ml / min

[0048] Raffinate flow rate: U R =1.8ml / min

[0049] Extraction flow rate: U E =2.0ml / min

[0050] Zone 1 velocity: U E =6.7ml / min

[0051] Switching time: t s =720s

[0052] b. Finished product analysis

[0053] The composition of raffinate and extract was analyzed by silica gel column. The purity and yield of δ-tocoph...

Embodiment 3

[0055] Simulated moving bed system CSEP _ 916 (Noel, Germany), equipped with 8 chromatographic columns (ID2×10cm), 2 in each zone, the chromatographic columns are filled with activated alumina, and the columns are packed by high-pressure wet method. The mobile phase was n-hexane / acetone solution (99 / 1, v / v), and the temperature was 30°C. The purity of the mixed tocopherols used for feeding is 97.5%, which contains 22.8% of α-tocopherol, 2.8% of β-tocopherol, 34.7% of γ-tocopherol and 37.2% of δ-tocopherol. mg / ml feed solution.

[0056] a. Operating conditions

[0057] Injection liquid flow rate: U F =1ml / min

[0058] Eluent flow rate: U D =3.1ml / min

[0059] Raffinate flow rate: U R =2.2ml / min

[0060] Extraction flow rate: U E =1.9ml / min

[0061] Zone 1 velocity: U E =6.9ml / min

[0062] Switching time: t s =708s

[0063] b. Finished product analysis

[0064] The composition of raffinate and extract was analyzed by silica gel column. The purity and yield of δ-t...

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PUM

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Abstract

The invention relates to a method for separating single tocopherol from mixed tocopherol, which takes the mixed tocopherol with a content of 50 percent to 100 percent as a raw material and adopts a four-area simulated moving bed chromatography system to separate a d-alpha-tocopherol, a d-beta-tocopherol, a d-gamma-tocopherol and a d-delta tocopherol with the purity and yield all more than 98 percent. As the simulated moving bed chromatography separation is a continuous process, the method has the advantages of high degree of production automation, simple technique, high production efficiency, continuous production and stable product quality. As an adsorbent and a solvent have low consumption, the whole separating device does not relate to chemical reactions.

Description

technical field [0001] The invention relates to chemical separation technology, in particular to a method for separating individual tocopherols from mixed tocopherols. Background technique [0002] Natural vitamin E (scientific name tocopherol) is a mixture mainly composed of four tocopherol homologues derived from tocol, including: d-α-, d-β-, d-γ- and d-delta-tocopherol, they all have saturated C16 side chains, and differ only in the number and position of methyl groups on the benzene ring. Although their structures are very similar, their biological activities are different, among which: d-α-tocopherol (activity is 100)>d-β-tocopherol (activity is 10-50)>d-γ-tocopherol (activity 10)>d-δ-tocopherol (activity 1). [0003] Natural vitamin E is widely used in medicine, cosmetics and food industry as an antioxidant and nutritional supplement. It is superior to synthetic vitamin E in terms of biological activity, nutritional physiological effects and use safety. How...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/72
Inventor 杨亦文吕裕斌任其龙吴平东苏宝根吴彩娟苏云黄梅
Owner ZHEJIANG UNIV
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