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A kind of decolorization purification method of vitamin E

A purification method and vitamin technology, which is 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, and failure to reduce viscosity, etc., to achieve obvious decolorization effect, lighter color, and lower viscosity. Effect

Active Publication Date: 2018-06-26
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] Take a sample of vitamin E (containing 84.20% tocopherol, of which 7.33% α-tocopherol, 0.97% β-tocopherol, 53.76% γ-tocopherol, 22.14% δ-tocopherol, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd. ) 30g, add 90g of absolute ethanol to dissolve, then add 9g of composite decolorizer (activated clay: activated carbon: diatomaceous earth: magnesium silicate = 100:50:50:30, w / w), stir and heat to 78°C for condensation Reflux and decolorize for 3h and filter. The filtrate was distilled under reduced pressure to remove ethanol to obtain a decolorized vitamin E product.

[0055] Take 50g of SephadexLH-20, add 300ml of chloroform:methanol=3:2(v / v) to fully swell, take 150ml of the swollen gel and load it into a chromatography column (2cm×50cm), and use it twice The column volume elution equilibrates the column. Take 0.3238g of the above decolorized vitamin E product, add 3ml of chloroform:methanol=3:2(v / v) to dissolve and load the sample. The column is eluted with ...

Embodiment 2

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

[0058] Take 200g of SephadexLH-20, add chloroform: methanol=3:1 (v / v) 1000mL to fully swell, take 700mL of swollen gel and load it into a chromatography column (3cm×100cm), and use 2 times The column volume elution equilibrates the column. Take 1.4889g of the above decolorized vitamin E product, add 10ml of chloroform:methanol=3:1 (v / v) to dissolve and load the sample. The column is eluted with chloroform:methanol=3:1 (v / v). The liquid was continuously collected and tested by thin-l...

Embodiment 3

[0060] Take vitamin E samples (containing 51.04% tocopherol, of which 12.33% α-tocopherol, β-tocopherol 1.89%, γ-tocopherol 32.36%, and δ-tocopherol 4.46%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd. ) 30g, add 60g of absolute ethanol to dissolve, then add 9g of composite decolorizing agent (activated clay: activated carbon: diatomaceous earth: magnesium silicate = 100:80:30:10, w / w), stir and heat to 80°C for condensation Reflux and decolorize for 2h and filter. The filtrate was distilled under reduced pressure to remove ethanol to obtain a decolorized vitamin E product.

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

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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, easily soluble in organic solvents such as ethanol, acetone, 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 homologs, namely α-tocopherol, α-tocotrienol, β-tocopherol, β-tocotrienol, and γ-tocopherol. Tocopherol, γ-tocotrienol, δ-tocopherol and δ-tocotrienol, of which α-tocopherol has the largest biological activity, and is effective when used as medicines and health products; δ-tocopherol has antioxidant activity 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 and has no optical rotation. [0003] Vitamin E is an essential n...

Claims

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Application Information

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Patent Type & Authority Patents(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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