Method for preparing natural alpha tocopherol and mixing tocopherol by one-step method

A natural technology of tocopherol, which is applied in the direction of pharmaceutical formulations, cosmetic preparations, dressing preparations, etc., can solve problems such as high α-tocopherol content, affecting product quality, and affecting use effects, so as to achieve high product quality and eliminate Residue of toxic organic solvents and the effect of using less equipment

Active Publication Date: 2014-11-05
山东圣地嘉禾生物工程有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this process is that a large amount of highly toxic organic solvents are used in the transformation process of mixed tocopherols, which is likely to affect product quality and cause safety hazards; at the same time, the original α-tocoph

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  • Method for preparing natural alpha tocopherol and mixing tocopherol by one-step method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] The method for preparing natural α-tocopherol and mixed tocopherol by one-step method comprises the following steps:

[0040] (1) Methyl esterification: Preheat 1Kg of soybean oil deodorized distillate to 40°C, slowly add 700ml of methanol reagent, add 5% concentrated sulfuric acid dropwise to the reactant while stirring, and control the reaction temperature at 66-68°C. The time is 3h;

[0041] (2) Washing: Add 80-85°C hot water to the above reaction solution, wash until the pH value of the water phase is greater than 5.0, let stand and separate and discard the water phase;

[0042] (3) Dissolving and filtering: add 500ml of ethanol solution to the organic phase, stir, slowly cool down to 10°C, let stand for 2h, and suction filter through a Buchner funnel to obtain 1640ml of tocopherol solution;

[0043] (4) Adsorption:

[0044] (a) Fluidized bed adsorption of solution: 1# resin column is loaded with 200ml of strong basic anion exchange resin, and 600ml of 1mol / L sodi...

Embodiment 2

[0051] The method for preparing natural α-tocopherol and mixed tocopherol by one-step method comprises the following steps:

[0052] (1) Methyl esterification: preheat 1Kg of corn oil deodorized distillate to 40°C, slowly add 500ml of methanol reagent, add 2% concentrated sulfuric acid dropwise to the reactant while stirring, and control the reaction temperature at 60-64°C. The reaction time is 3h;

[0053] (2) Washing: Add 80-85°C hot water to the above reaction solution, wash until the pH value of the water phase is greater than 5.0, let stand and separate and discard the water phase;

[0054] (3) Dissolving and filtering: add 200ml of ethanol solution to the organic phase, stir, slowly cool down to 5°C, let stand for 2h, and suction filter with Buchner funnel to obtain 1240ml of tocopherol solution;

[0055] (4) Adsorption:

[0056] (a) Fluidized bed adsorption of solution: 1# resin column is loaded with 250ml of strong basic anion exchange resin, and 750ml of 1mol / L sodi...

Embodiment 3

[0063] The method for preparing natural α-tocopherol and mixed tocopherol by one-step method comprises the following steps:

[0064] (1) methyl esterification: get rapeseed oil deodorization distillate 700g, olive oil deodorization distillate 300g and preheat to 35 ℃, slowly add 1000ml methanol reagent, add dropwise 6% concentrated sulfuric acid in the reactant under the stirring situation, The reaction temperature is controlled at 68-70°C, and the reaction time is 2h;

[0065] (2) Washing: Add 80-85°C hot water to the above reaction solution, wash until the pH value of the water phase is greater than 5.0, let stand and separate and discard the water phase;

[0066] (3) Dissolution and filtration: add 1000ml of ethanol solution to the organic phase, stir, slowly cool down to 25°C, let stand for 2h, and filter through Buchner funnel to obtain 2404ml of tocopherol solution;

[0067] (4) Adsorption:

[0068] (a) Fluidized bed adsorption of solution: 1# resin column is loaded wi...

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Abstract

The invention discloses a method for preparing natural alpha tocopherol and mixing tocopherol by a one-step method, which relates to the technical field of separation and extraction in bioengineering. The method comprises the following steps: performing esterification of plant oil deodorizer distillate; washing; dissolving and filtering tocopherol; adsorbing a fluidized bed of a tocopherol solution by resin; dynamically absorbing a tocopherol adsorption waste liquid by resin; desorpting, and performing molecular distillation to obtain the alpha tocopherol and mixing tocopherol. According to the invention, no organic solvent is used for the alpha tocopherol, and alpha tocopherol has the advantages of environmental protection and safety, and has the characteristics of green and health by comparing with the alpha tocopherol prepared by a traditional method; and the produced mixing tocopherol has the characteristics of high quality, high yield, low cost, and easy batch production.

Description

technical field [0001] The invention belongs to the technical field of separation and extraction in bioengineering, and in particular relates to a method for preparing natural α-tocopherol and mixed tocopherol in one step. Background technique [0002] Natural vitamin E, also known as natural tocopherol, is one of the earliest vitamins discovered by humans. Tocopherol was discovered by Evans et al. from wheat germ extract in 1922. Tocopherol is a substance that can affect the reproductive ability of animals, so it was named "anti-sterility vitamin". In 1938, American E. Fernholz described the molecular formula of biologically active natural tocopherol in his paper. In the same year, P.vonKarrer and H.Fritzsche and others successfully synthesized biologically active tocopherol composed of different diastereoisomers for the first time. In the 1980s, natural tocopherol became popular all over the world, and many countries such as the United States, Germany, and Japan develope...

Claims

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Application Information

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IPC IPC(8): C07D311/72A23L3/3544
CPCC07D311/72A23L3/3544A61K8/678A61Q19/08
Inventor 朱雷常晓菲左良成张伟李若坤
Owner 山东圣地嘉禾生物工程有限公司
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