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Method for preparing low-benzopyrene high-purity d-alpha tocopherol acetate

A technology of tocopheryl acetate and benzopyrene, which is applied in organic chemistry and other fields, and can solve the problems of purity or benzopyrene not meeting EU standards.

Inactive Publication Date: 2012-05-02
浙江伊宝馨生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] European and American countries have very strict requirements on d-α-tocopheryl acetate, but most of the current domestic processes use traditional methods, and the produced d-α-tocopheryl acetate cannot meet the EU standards in terms of purity or benzopyrene.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Take 100 grams of d-alpha tocopherol, mix it with 300 grams of n-hexane and 4 grams of zinc chloride, control the temperature at 35°C, slowly add acetic anhydride dropwise into the reaction kettle, carry out esterification for 2 hours, wash with water, and concentrate to obtain d - the crude product of α-tocopherol acetate, then mix the crude product with 400 grams of ethanol, put it on the column, control the flow rate of the upper column, and the temperature is 20-50°C, absorb it through the D-101 type macroporous adsorption resin, and concentrate and desolventize the effluent, The concentrate is then mixed with 400 grams of ethanol, 5 grams of activated carbon is added, and at a constant temperature of 60°C, the external circulation method is adopted for 2 hours, filtered and concentrated, and the concentrate is then purified by short-range molecular distillation under high vacuum conditions. , to obtain the finished product of d-alpha tocopheryl acetate. The measure...

Embodiment 2

[0021] Take 100 grams of d-alpha tocopherol, mix it with 300 grams of petroleum ether and 5 grams of zinc chloride, control the temperature at 35°C, slowly add acetic anhydride dropwise into the reaction kettle, carry out esterification for 2 hours, wash with water, and concentrate to obtain d - α-tocopherol acetate crude product, then the crude product is mixed with 400 grams of ethanol, put on the column, control the flow rate of the upper column, the temperature is 20 ~ 50 ℃, absorb through AB-8 type macroporous adsorption resin, the effluent is concentrated and desolvated, The concentrate is then mixed with 400 grams of ethanol, 5 grams of activated carbon is added, and at a constant temperature of 60°C, the external circulation method is adopted for 2 hours, filtered and concentrated, and the concentrate is then purified by short-range molecular distillation under high vacuum conditions. , to obtain the finished product of d-alpha tocopheryl acetate. The measured content ...

Embodiment 3

[0023] Take 100 grams of d-alpha tocopherol, mix it with 400 grams of n-hexane and 4 grams of zinc chloride, control the temperature at 35°C, slowly add acetic anhydride dropwise into the reaction kettle, carry out esterification for 2 hours, wash with water, and concentrate to obtain d -The crude product of α-tocopherol acetate, then mix the crude product with 400 grams of anhydrous methanol and ethanol mixture (volume ratio 1:2), put it on the column, control the flow rate of the upper column, and the temperature is 20-50°C, and pass through DA-201 Type macroporous adsorption resin for adsorption, the effluent is concentrated and desolvated, the concentrated solution is mixed with 400 grams of ethyl acetate, 5 grams of activated carbon is added, and at a constant temperature of 60 ° C, an external circulation method is adopted for 2 hours, filtered and concentrated. The concentrated solution is then purified by short-range molecular distillation under high vacuum conditions t...

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Abstract

The invention discloses a method for preparing low-benzopyrene high-purity d-alpha tocopherol acetate. The method comprises the following steps of: mixing d-alpha tocopherol, an inert organic solvent and a catalyst in a certain ratio, controlling the temperature, performing esterification reaction on the mixture and acetic anhydride, mixing obtained crude d-alpha tocopherol acetate and a polar solvent, loading to a column, adsorbing by using resin so as to remove impurities, mixing the obtained product and the inert organic solvent, adding a removal agent in a certain ratio, circulating at the constant temperature of 60 DEG C for 2 hours in an external circulation mode, filtering, concentrating, desolventizing, and performing short-path molecular distillation refinement under high vacuum conditions to obtain the low-benzopyrene high-purity d-alpha tocopherol acetate. The content of the obtained product is high, and the content of the d-alpha tocopherol acetate is more than or equal to 98 percent; the specific rotation is more than or equal to +24 degrees; the concentration of heavy metals (based on Pb) is less than or equal to 10ppm; and the concentration of benzopyrene is less than or equal to 2ppb. The quality of products meets the standards established by developed countries in Europe and America.

Description

technical field [0001] The invention relates to the technical field of natural food additive production, in particular to a preparation method of low-benzopyrene and high-purity d-alpha tocopheryl acetate. Background technique [0002] Vitamin E (referred to as VE) has important physiological functions and is an essential nutrient for the human body. It is widely used in pharmaceuticals, health care products, beauty and skin care products, food and feed additives and other industries. [0003] Natural VE has four homologues, which are called α-tocopherol, β-tocopherol, γ-tocopherol and δ-tocopherol. They all have the commonality of natural VE, but also show different personalities, so they are differentiated in terms of functions and applicable fields. The α-type monomer has the largest biological activity, and has the best drug effect when used as medicine and health care product. [0004] d-alpha tocopherol acetate is one of the derivatives of d-alpha tocopherol, which c...

Claims

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Application Information

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IPC IPC(8): C07D311/72
Inventor 黄茂清陆定贤
Owner 浙江伊宝馨生物科技股份有限公司
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