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Decoloration and purification method for vitamin E

A purification method and vitamin technology, applied in the field of decolorization and purification of vitamin E, can solve the problems of no obvious improvement in product purity, unsatisfactory purification effect, failure to reduce viscosity, etc., and achieve obvious decolorization effect, light color, and viscosity reduction. Effect

Active Publication Date: 2016-05-18
WILMAR SHANGHAI BIOTECH RES & DEV CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the above-mentioned decolorization method, although there is a certain decolorization effect, there are still some deficiencies: if activated carbon or activated clay is used to process, the color of the product becomes lighter, but the product fails to reduce viscosity and improve fluidity, and for the purity of the product There is no obvious improvement; if normal phase silica gel is used as the chromatographic medium for decolorization, relatively high losses will be caused due to the adsorption between the product and silica gel, and the regeneration of normal phase silica gel is also a problem; although macroporous resin treatment has certain The decolorization effect, but the purification effect is not ideal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Vitamin E samples (containing 84.20% of tocopherol, including 7.33% of α-tocopherol, 0.97% of β-tocopherol, 53.76% of γ-tocopherol and 22.14% of δ-tocopherol were purchased from Jiangsu Spring Valley Biological Products Co., Ltd. ) 30g, add 90g dehydrated ethanol to dissolve, then add 9g composite decolorizing agent (activated clay: activated carbon: diatomaceous earth: magnesium silicate=100:50:50:30, w / w), be heated to 78 ℃ of condensation after stirring Reflux for decolorization for 3h and filter. Ethanol was distilled off from the filtrate under reduced pressure to obtain the decolorized vitamin E product.

[0055] Take 50g SephadexLH-20 Sephadex, add 300ml of chloroform:methanol=3:2 (v / v) to fully swell, take 150ml of the swollen gel and put it into a chromatography column (2cm×50cm), and use 2 times Column Volume Elution equilibrates the column. Take 0.3238g of the above-mentioned decolorized vitamin E product, add 3ml of chloroform:methanol=3:2(v / v) to dissolve...

Embodiment 2

[0057] Get vitamin E sample (containing α-tocopherol 91.42%, purchased from Jiangsu Spring Valley Biological Products Co., Ltd.) 30g, add 95% ethanol 90g to dissolve, then add 6g composite decolorizing agent (activated clay: activated carbon: diatomaceous earth: silicic acid Magnesium=100:70:50:30, w / w), heated to 78°C after stirring, condensed and refluxed for 3 hours for decolorization, and filtered. Ethanol was distilled off from the filtrate under reduced pressure to obtain the decolorized vitamin E product.

[0058] Take 200g SephadexLH-20 Sephadex, add chloroform:methanol=3:1 (v / v) 1000mL to fully swell, take 700mL of the swollen gel and put it into a chromatography column (3cm×100cm), and use 2 times Column Volume Elution equilibrates the column. Take 1.4889g of the above-mentioned decolorized vitamin E product, add 10ml of chloroform:methanol=3:1 (v / v) to dissolve and apply the sample, the chromatographic column is eluted with chloroform:methanol=3:1 (v / v), and the el...

Embodiment 3

[0060] Vitamin E samples (containing 51.04% of tocopherol, including 12.33% of α-tocopherol, 1.89% of β-tocopherol, 32.36% of γ-tocopherol and 4.46% of δ-tocopherol were purchased from Jiangsu Spring Valley Biological Products Co., Ltd. ) 30g, add 60g absolute ethanol to dissolve, then add 9g composite decolorizing agent (activated clay: activated carbon: diatomaceous earth: magnesium silicate=100:80:30:10, w / w), be heated to 80 ℃ of condensation after stirring Reflux for decolorization for 2h and filter. Ethanol was distilled off from the filtrate under reduced pressure to obtain the decolorized vitamin E product.

[0061]Take 100g SephadexLH-20 Sephadex, add dichloromethane:methanol=3:1 (v / v) 500ml to fully swell, take 300ml of the swollen gel and put it into a chromatography column (2.5cm×70cm), And elute with 2 times the column volume to equilibrate the chromatographic column. Take 0.6238g of the above-mentioned decolorized vitamin E product, add 5ml of dichloromethane:m...

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Abstract

The invention provides a decoloration and purification method for vitamin E. The method includes the following steps: (a) providing a composite decoloration agent to perform decoloration to a vitamin E product; (b) eluting the decolored vitamin E in the step (a) through column chromatography by means of an eluting agent, and collecting an eluent component; and (c) concentrating the eluent component in the step (b) to prepare the decolored and purified vitamin E. In the step (a), the composite decoloration agent includes activated clay, activated carbon, diatomite and magnesium silicate according to 100:50-100:30-70:10-50 by mass. The decoloration and purification method can shallow the color and reduce the viscosity of vitamin E, thereby improving flowability and also increasing the purity of the vitamin E. The vitamin E is low in loss and has a high recovery rate during the decoloration and purification.

Description

technical field [0001] The invention relates to a method for decolorizing and purifying vitamin E. Background technique [0002] Vitamin E, also known as tocopherol, is a fat-soluble vitamin that is easily soluble in organic solvents such as ethanol, acetone, and n-hexane, and has a good antioxidant effect. Vitamin E is divided into natural vitamin E and synthetic vitamin E. Natural vitamin E generally contains eight homologues, namely α-tocopherol, α-tocotrienol, β-tocopherol, β-tocotrienol, γ- Tocopherol, γ-tocotrienol, δ-tocopherol and δ-tocotrienol, among which α-tocopherol has the highest biological activity, and has better effect when used as medicine and health care products; the antioxidant activity of δ-tocopherol The strongest, especially suitable for food and cosmetics as an antioxidant. Natural vitamin E has dextrorotatory optical activity, while synthetic vitamin E is a racemate composed of various optical isomers without optical activity. [0003] Vitamin E ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/72B01J20/20
Inventor 张戈黄贤校高媛媛邹彦平
Owner WILMAR SHANGHAI BIOTECH RES & DEV CENT
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