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Separation and purification method of d-delta-tocopherol

A purification method and technology of tocopherol, which is applied in the field of separation and purification of d-δ-tocopherol, can solve the problems of inability to realize industrialization, large resin and solvent, difficult industrial application, etc., and achieve good separation and purification effect and low equipment requirements , the effect of increasing the yield

Active Publication Date: 2014-12-24
NINGBO DAHONGYING BIO ENG
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

U.S. patents US 3122565, US 3402183, and US 2005 / 131240 all use ion exchange resins to separate tocopherols, and obtain high-purity D-α-tocopherols, D-γ-tocopherols, and D-δ-tocopherols. Phenol homologues have very little structural difference, consume a large amount of resin and solvent, and the separation cost is too high to realize industrialization; U.S. Patents US 4480108, US 4602098, US 4607111, etc. are based on D-α-tocopherol, D-β-tocopherol , D-γ-tocopherol and D-δ-tocopherol ester derivatives have different degrees of difficulty in the deacylation reaction, and the deacylation reaction is combined with chromatographic separation or distillation to achieve the separation of each tocopherol homolog
This type of method does not directly use tocopherol as the raw material for separation, and the process is relatively complicated, so it is not easy for industrial application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh 20g of high-content mixed tocopherol concentrate (the high-content mixed tocopherol concentrate is obtained by preparation, preparation method: use DD oil as raw material, obtain mixed tocopherol concentrate by molecular distillation and ion exchange adsorption, the mixed tocopherol concentrate The content of tocopherol in the tocopherol concentrated solution is 30%), add 20ml n-hexane, be heated to fully dissolved, transfer the tocopherol solution to the top of the column that 200g of silica gel is housed, make it slowly flow through the silica gel column, until all the solutions are completely dissolved Completely adsorbed on the silica gel column, add 1BV (column volume) n-hexane to elute, then use 0.5BV of 3% tetrahydrofuran-n-hexane mixed eluent to elute the column, and then further increase the polarity of the mixed solvent, add 0.5BV 8% tetrahydrofuran-n-hexane mixed eluent to elute the column; in the above process, the eluent was collected in sections, and ...

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Abstract

The invention discloses a separation and purification method of d-delta-tocopherol. According to the method, a silica gel column chromatography process is combined with a resin ion exchange adsorption process, and ion exchange resin is subjected to CO2 desorption, so that the yield of d-delta-tocopherol is effectively increased. The method is relatively low in equipment requirement, low in energy consumption and suitable for industrialization.

Description

technical field [0001] The invention belongs to the field of chemical engineering, and in particular relates to a method for separating and purifying d-delta-tocopherol. Background technique [0002] Natural vitamin E is a mixture mainly composed of four tocopherol homologues derived from tocols, including d-alpha-tocopherol, d-beta-tocopherol, d-gamma-tocopherol, and d- delta-tocopherol, both of which are saturated with C 16 The side chains differ only in the number and position of the methyl groups on the benzene ring. Although their structures are very similar, their biological activities are different, respectively d-α-tocopherol>d-β-tocopherol>d-γ-tocopherol>d-δ-tocopherol, and the antioxidant activity is d - the highest level of δ-tocopherol, d-β-, d-γ- and d-δ-tocopherol can be converted into d-α-tocopherol by chemical transformation method, so as to obtain high-purity concentrated d-α-tocopherol liquid. However, the separation and purification of d-δ-toc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/72
CPCC07D311/72
Inventor 张源仁肖翔章生魏国华
Owner NINGBO DAHONGYING BIO ENG
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