CN102432583A - Method for preparing low-benzopyrene high-purity d-alpha tocopherol acetate - Google Patents
Method for preparing low-benzopyrene high-purity d-alpha tocopherol acetate Download PDFInfo
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- CN102432583A CN102432583A CN201110326968XA CN201110326968A CN102432583A CN 102432583 A CN102432583 A CN 102432583A CN 201110326968X A CN201110326968X A CN 201110326968XA CN 201110326968 A CN201110326968 A CN 201110326968A CN 102432583 A CN102432583 A CN 102432583A
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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
The present invention relates to the natural additive for foodstuff production technical field, be specifically related to the preparation method of the low highly purified d-alpha-tocopherol of benzopyrene acetic ester.
Background technology
Vitamin E (being called for short VE) has the important physical function, is the nutrient substance of needed by human, is widely used in industries such as medicine, healthcare products, cosmetics and skincare product, food and feed additive.
Natural VE has four kinds of homologues, is called alpha-tocopherol, 5,8-dimethyl tocol, Gamma-Tocopherol and Delta-Tocopherol respectively.They all have the general character of natural VE, show the individual character that has nothing in common with each other again, therefore on function and suitable application area, appear differential.The monomeric biological activity of α type is maximum, and drug effect is best as medicine and healthcare products the time.
D-alpha-tocopherol acetic ester is one of derived product of d-alpha-tocopherol, and it has continued the biological activity of d-alpha-tocopherol.D-alpha-tocopherol acetic ester is the main raw material of various VE protective foodss, can be used as the midbody of synthesizing water-soluble vitamin E.Though the antioxidant property of free VE is apparently higher than the VE ester derivative, because VE ester class is very easy to therefore added the food or the healthcare products of VE ester class by the lipase-catalyzed VE that dissociates accordingly that is hydrolyzed into, its VE performance does not receive any infringement.The VE ester derivative is applied in a series of industries such as foodstuff additive, medicine, makeup, animal-feed, nutrition-fortifying agent, towards domestic and international huge VE market, enlarges the research for application and development of VE, and the development of VE derived product is seemed very urgent.
American-European countries is very harsh to the requirement of d-alpha-tocopherol acetic ester, but at present domestic technology is used traditional method mostly, and the d-alpha-tocopherol acetic ester purity of being produced still is that the index of benzopyrene does not all reach European Union's standard.
Summary of the invention
The quality index that the technical problem that the present invention will solve provides a kind of products obtained therefrom can reach the preparation method of the highly purified d-alpha-tocopherol of the low benzopyrene acetic ester of European Union member countries' standard.
For realizing above-mentioned purpose, technical scheme of the present invention is:
The d-alpha-tocopherol is mixed with inert organic solvents, catalyzer in certain proportion, and controlled temperature carries out esterification with aceticanhydride, and the d-alpha-tocopherol acetic ester bullion that obtains mixes with polar solvent again; Upper prop through resin absorption, is removed impurity, mixes with inert organic solvents again; Add a certain proportion of agent that removes, under 60 ℃ of temperature constant temperature, adopt the outer circulation mode, circulated 2 hours; Filter, concentrate precipitation, last under the condition of high vacuum, carry out that short-range molecular distillation is refining promptly to be got.
The preparation method of the low highly purified d-alpha-tocopherol of benzopyrene acetic ester may further comprise the steps:
(A) the d-alpha-tocopherol is mixed with inert organic solvents, catalyzer in certain proportion; About 35 ℃ of controlled temperature, slowly aceticanhydride is added dropwise in the reaction kettle, carries out esterification about 2 hours; Reaction finishes water flush away catalyzer, concentrates then and obtains d-alpha-tocopherol acetic ester bullion; Described inert organic solvents is any in normal hexane, the sherwood oil; Described d-alpha-tocopherol and inert organic solvents blending ratio are 1: 3-5; Described catalyzer is any in zinc chloride, the aluminum chloride; Described catalyzer dosage is in d-alpha-tocopherol weight 3-5%;
(B) d-alpha-tocopherol acetic ester bullion is mixed with polar solvent according to a certain percentage; Upper prop, control upper prop flow, temperature are 20～50 ℃, through resin absorption; With weakly acidic organic impurity absorption, effluent obtains the higher d-alpha-tocopherol acetic ester bullion of purity after concentrating precipitation; Described polar solvent be in anhydrous methanol, ethanol, the Virahol any or plant arbitrarily and mix with arbitrary proportion; Described d-alpha-tocopherol acetic ester bullion and polar solvent blending ratio are 1: 3-5; Described upper prop flow is 1%～5% of a resin volume for the PM add-on; Described resin is any in D-101 type macroporous adsorbent resin, AB-8 type macroporous adsorbent resin, DA-201 type macroporous adsorbent resin, X-5 type macroporous adsorbent resin, DM130 macroporous adsorbent resin, the DM-301 type macroporous adsorbent resin;
(C) above-mentioned purity is higher d-alpha-tocopherol acetic ester bullion mixes with inert organic solvents, adds a certain proportion of agent that removes, and under 60 ℃ of temperature constant temperature, adopts the outer circulation mode, circulates 2 hours, filters to remove to remove agent, concentrates precipitation; Described inert organic solvents be in ethanol, methyl acetate, ETHYLE ACETATE, propyl acetate, butylacetate, the Virahol any or plant arbitrarily and mix with arbitrary proportion; Described d-alpha-tocopherol acetic ester bullion and inert organic solvents blending ratio are 1: 3-5; It is described that to remove agent be a kind of or any kind mix with arbitrary proportion in gac, silica gel, atlapulgite, the molecular sieve; It is best that to remove agent be that gac, silica gel any or two kinds mix with arbitrary proportion; The described agent dosage that removes is in d-alpha-tocopherol acetic ester bullion weight 4-6%;
(D) with the d-alpha-tocopherol acetic ester behind the above-mentioned concentrated precipitation under the condition of high vacuum, it is refining to carry out short-range molecular distillation, promptly obtains the low highly purified d-alpha-tocopherol of benzopyrene acetic ester finished product.
100 gram d-alpha-tocopherols can obtain d-alpha-tocopherol acetic ester bullion or the about 100-105 gram of d-alpha-tocopherol acetic ester finished product.
The preparation method of the highly purified d-alpha-tocopherol of low benzopyrene of the present invention acetic ester, products obtained therefrom content is high, d-alpha-tocopherol acetate content>=98%; Specific rotatory power>=+24 °; Heavy metal (in Pb)≤10ppm; Benzopyrene≤2ppb.
Quality product has reached the standard that American-European developed country formulates.
Embodiment
Below in conjunction with embodiment the present invention is further described, following each embodiment only is used to explain the present invention, but to not restriction of the present invention.
Embodiment one
Get d-alpha-tocopherol 100 grams, mix with 300 gram normal hexanes and 4 gram zinc chloride, 35 ℃ of controlled temperature slowly are added dropwise to aceticanhydride in the reaction kettle; Carried out esterification 2 hours, washing, concentrated obtains d-alpha-tocopherol acetic ester bullion, this bullion and 400 gram ethanol is mixed again; Upper prop, control upper prop flow, temperature are 20～50 ℃, through D-101 type absorption with macroporous adsorbent resin, effluent concentrates precipitation; Liquid concentrator mixes with 400 gram ethanol again, adds 5 gram gacs, under 60 ℃ of temperature constant temperature; Adopt the outer circulation mode, circulated 2 hours, filter, concentrate; This liquid concentrator under the condition of high vacuum, carries out short-range molecular distillation and makes with extra care again, obtains d-alpha-tocopherol acetic ester finished product.Record d-alpha-tocopherol acetate content 98.3%; Specific rotatory power+24.2 °; Heavy metal (in Pb) 9.5ppm; Benzopyrene≤2ppb.
Embodiment two
Get d-alpha-tocopherol 100 grams, mix with 300 gram sherwood oils and 5 gram zinc chloride, 35 ℃ of controlled temperature slowly are added dropwise to aceticanhydride in the reaction kettle; Carried out esterification 2 hours, washing, concentrated obtains d-alpha-tocopherol acetic ester bullion, this bullion and 400 gram ethanol is mixed again; Upper prop, control upper prop flow, temperature are 20～50 ℃, through AB-8 type absorption with macroporous adsorbent resin, effluent concentrates precipitation; Liquid concentrator mixes with 400 gram ethanol again, adds 5 gram gacs, under 60 ℃ of temperature constant temperature; Adopt the outer circulation mode, circulated 2 hours, filter, concentrate; This liquid concentrator under the condition of high vacuum, carries out short-range molecular distillation and makes with extra care again, obtains d-alpha-tocopherol acetic ester finished product.Record d-alpha-tocopherol acetate content 98.2%; Specific rotatory power+24.3 °; Heavy metal (in Pb) 9.7ppm; Benzopyrene≤2ppb.
Embodiment three
Get d-alpha-tocopherol 100 grams, mix with 400 gram normal hexanes and 4 gram zinc chloride, 35 ℃ of controlled temperature slowly are added dropwise to aceticanhydride in the reaction kettle; Carried out esterification 2 hours, washing, concentrated obtains d-alpha-tocopherol acetic ester bullion, this bullion is mixed with 400 gram anhydrous methanols, alcohol mixeding liquid (volume ratio 1: 2) again; Upper prop, control upper prop flow, temperature are 20～50 ℃, through DA-201 type absorption with macroporous adsorbent resin, effluent concentrates precipitation; Liquid concentrator mixes with 400 gram ETHYLE ACETATE again, adds 5 gram gacs, under 60 ℃ of temperature constant temperature; Adopt the outer circulation mode, circulated 2 hours, filter, concentrate; This liquid concentrator under the condition of high vacuum, carries out short-range molecular distillation and makes with extra care again, obtains d-alpha-tocopherol acetic ester finished product.Record d-alpha-tocopherol acetate content 98.4%; Specific rotatory power+24.1 °; Heavy metal (in Pb) 9.4ppm; Benzopyrene≤2ppb.
Embodiment four
Get d-alpha-tocopherol 100 grams, mix with 400 gram normal hexanes and 5 gram zinc chloride, 35 ℃ of controlled temperature slowly are added dropwise to aceticanhydride in the reaction kettle; Carried out esterification 2 hours, washing, concentrated obtains d-alpha-tocopherol acetic ester bullion, this bullion is mixed with 400 gram anhydrous methanols, alcohol mixeding liquid (volume ratio 1: 3) again; Upper prop, control upper prop flow, temperature are 20～50 ℃, through DA-201 type absorption with macroporous adsorbent resin, effluent concentrates precipitation; Liquid concentrator mixes with 400 gram ethanol, 50 gram methyl acetates again, adds 5 gram silica gel, under 60 ℃ of temperature constant temperature; Adopt the outer circulation mode, circulated 2 hours, filter, concentrate; This liquid concentrator under the condition of high vacuum, carries out short-range molecular distillation and makes with extra care again, obtains d-alpha-tocopherol acetic ester finished product.Record d-alpha-tocopherol acetate content 98.1%; Specific rotatory power+24.1 °; Heavy metal (in Pb) 9.6ppm; Benzopyrene≤2ppb.
Embodiment five
Get d-alpha-tocopherol 100 grams, mix with 500 gram sherwood oils and 5 gram aluminum chloride, 35 ℃ of controlled temperature slowly are added dropwise to aceticanhydride in the reaction kettle; Carried out esterification 2 hours, washing, concentrated obtains d-alpha-tocopherol acetic ester bullion, this bullion is mixed with 400 gram anhydrous methanols, alcohol mixeding liquid (volume ratio 1: 2) again; Upper prop, control upper prop flow, temperature are 20～50 ℃, through X-5 type absorption with macroporous adsorbent resin, effluent concentrates precipitation; Liquid concentrator mixes with 400 gram ethanol, 50 gram butylacetates again, adds 3 gram gacs and 2 gram silica gel, under 60 ℃ of temperature constant temperature; Adopt the outer circulation mode, circulated 2 hours, filter, concentrate; This liquid concentrator under the condition of high vacuum, carries out short-range molecular distillation and makes with extra care again, obtains d-alpha-tocopherol acetic ester finished product.Record d-alpha-tocopherol acetate content 98.2%; Specific rotatory power+24.1 °; Heavy metal (in Pb) 9.9ppm; Benzopyrene≤2ppb.
Embodiment six
Get d-alpha-tocopherol 100 grams, mix with 300 gram sherwood oils and 5 gram aluminum chloride, 35 ℃ of controlled temperature slowly are added dropwise to aceticanhydride in the reaction kettle; Carried out esterification 2 hours, washing, concentrated obtains d-alpha-tocopherol acetic ester bullion, this bullion and 400 gram anhydrous methanols, ethanol, Virahol mixed solution (volume ratio 1: 2: 1) is mixed again; Upper prop, control upper prop flow, temperature are 20～50 ℃, through DM-301 type absorption with macroporous adsorbent resin, effluent concentrates precipitation; Liquid concentrator mixes with 200 gram ethanol, 200 gram ETHYLE ACETATE, 50 gram propyl acetates again, adds 3 gram gacs, 2 gram silica gel and 1 gram atlapulgite, under 60 ℃ of temperature constant temperature; Adopt the outer circulation mode, circulated 2 hours, filter, concentrate; This liquid concentrator under the condition of high vacuum, carries out short-range molecular distillation and makes with extra care again, obtains d-alpha-tocopherol acetic ester finished product.Record d-alpha-tocopherol acetate content 98.3%; Specific rotatory power+24.2 °; Heavy metal (in Pb) 9.7ppm; Benzopyrene≤2ppb.
Embodiment seven
Get d-alpha-tocopherol 150 grams, mix with 500 gram normal hexanes and 5 gram aluminum chloride, 35 ℃ of controlled temperature slowly are added dropwise to aceticanhydride in the reaction kettle; Carried out esterification 2 hours, washing, concentrated obtains d-alpha-tocopherol acetic ester bullion, this bullion and 400 gram anhydrous methanols, ethanol, Virahol mixed solution (volume ratio 1: 3: 2) is mixed again; Upper prop, control upper prop flow, temperature are 20～50 ℃, through DA-201 type absorption with macroporous adsorbent resin, effluent concentrates precipitation; Liquid concentrator mixes with 200 gram ethanol, 100 gram ETHYLE ACETATE and 150 gram Virahols again, adds 3 gram gacs, 2 gram silica gel and 1 mol sieve, under 60 ℃ of temperature constant temperature; Adopt the outer circulation mode, circulated 2 hours, filter, concentrate; This liquid concentrator under the condition of high vacuum, carries out short-range molecular distillation and makes with extra care again, obtains d-alpha-tocopherol acetic ester finished product.Record d-alpha-tocopherol acetate content 98.4%; Specific rotatory power+24.1 °; Heavy metal (in Pb) 9.8ppm; Benzopyrene≤2ppb.
Embodiment eight
Get d-alpha-tocopherol 100 grams, mix with 500 gram normal hexanes and 5 gram zinc chloride, 35 ℃ of controlled temperature slowly are added dropwise to aceticanhydride in the reaction kettle; Carried out esterification 2 hours, washing, concentrated obtains d-alpha-tocopherol acetic ester bullion, this bullion and 400 gram anhydrous methanols, ethanol, Virahol mixed solution (volume ratio 1: 3: 1) is mixed again; Upper prop, control upper prop flow, temperature are 20～50 ℃, through X-5 type absorption with macroporous adsorbent resin, effluent concentrates precipitation; Liquid concentrator mixes with 200 gram ethanol, 100 gram ETHYLE ACETATE and 150 gram Virahols again, adds 1 gram gac, 3.5 gram silica gel and 1 mol sieve, under 60 ℃ of temperature constant temperature; Adopt the outer circulation mode, circulated 2 hours, filter, concentrate; This liquid concentrator under the condition of high vacuum, carries out short-range molecular distillation and makes with extra care again, obtains d-alpha-tocopherol acetic ester finished product.Record d-alpha-tocopherol acetate content 98.2%; Specific rotatory power+24.0 °; Heavy metal (in Pb) 9.9ppm; Benzopyrene≤2ppb.
Embodiment nine
Get d-alpha-tocopherol 150 grams, mix with 500 gram normal hexanes and 5 gram aluminum chloride, 35 ℃ of controlled temperature slowly are added dropwise to aceticanhydride in the reaction kettle; Carried out esterification 2 hours, washing, concentrated obtains d-alpha-tocopherol acetic ester bullion; Again this bullion is mixed with 400 gram anhydrous methanols, ethanol, Virahol mixed solution (volume ratio 1: 3: 1), upper prop, control upper prop flow, temperature are 20～50 ℃; Through X-5 type absorption with macroporous adsorbent resin, effluent concentrates precipitation, and liquid concentrator mixes with 200 gram ethanol, 100 gram propyl acetates and 150 gram Virahols again; Add 3 gram gacs, 1 gram silica gel and 1 gram atlapulgite, 0.5 mol sieve is under 60 ℃ of temperature constant temperature; Adopt the outer circulation mode, circulated 2 hours, filter, concentrate; This liquid concentrator under the condition of high vacuum, carries out short-range molecular distillation and makes with extra care again, obtains d-alpha-tocopherol acetic ester finished product.Record d-alpha-tocopherol acetate content 98.3%; Specific rotatory power+24.1 °; Heavy metal (in Pb) 9.9ppm; Benzopyrene≤2ppb.
Embodiment ten
Get d-alpha-tocopherol 150 grams, mix with 500 gram normal hexanes and 5 gram zinc chloride, 35 ℃ of controlled temperature slowly are added dropwise to aceticanhydride in the reaction kettle; Carried out esterification 2 hours, washing, concentrated obtains d-alpha-tocopherol acetic ester bullion, this bullion and 450 gram anhydrous methanols, ethanol, Virahol mixed solution (volume ratio 1: 3: 1) is mixed again; Upper prop, control upper prop flow, temperature are 20～50 ℃, through the AB-8 absorption with macroporous adsorbent resin, effluent concentrates precipitation; Liquid concentrator mixes with 300 gram ethanol, 100 gram ETHYLE ACETATE and 50 gram Virahols again, adds 2 gram gacs, 2 gram silica gel and 1 gram atlapulgite, and 0.5 mol sieve is under 60 ℃ of temperature constant temperature; Adopt the outer circulation mode, circulated 2 hours, filter, concentrate; This liquid concentrator under the condition of high vacuum, carries out short-range molecular distillation and makes with extra care again, obtains d-alpha-tocopherol acetic ester finished product.Record d-alpha-tocopherol acetate content 98.4%; Specific rotatory power+24.2 °; Heavy metal (in Pb) 9.8ppm; Benzopyrene≤2ppb.
Embodiment 11
Get d-alpha-tocopherol 100 grams, mix with 500 gram normal hexanes and 5 gram zinc chloride, 35 ℃ of controlled temperature slowly are added dropwise to aceticanhydride in the reaction kettle; Carried out esterification 2 hours, washing, concentrated obtains d-alpha-tocopherol acetic ester bullion, this bullion and 450 gram anhydrous methanols, ethanol, Virahol mixed solution (volume ratio 2: 2: 1) is mixed again; Upper prop, control upper prop flow, temperature are 20～50 ℃, through the DM-301 absorption with macroporous adsorbent resin, effluent concentrates precipitation; Liquid concentrator mixes with 300 gram ethanol, 100 gram ETHYLE ACETATE and 50 gram propyl acetates again, adds 4 gram gacs, 0.5 gram silica gel and 1.5 gram atlapulgites, under 60 ℃ of temperature constant temperature; Adopt the outer circulation mode, circulated 2 hours, filter, concentrate; This liquid concentrator under the condition of high vacuum, carries out short-range molecular distillation and makes with extra care again, obtains d-alpha-tocopherol acetic ester finished product.Record d-alpha-tocopherol acetate content 98.2%; Specific rotatory power+24.2 °; Heavy metal (in Pb) 9.7ppm; Benzopyrene≤2ppb.
Embodiment 12
Get d-alpha-tocopherol 150 grams, mix with 450 gram normal hexanes and 5 gram aluminum chloride, 35 ℃ of controlled temperature slowly are added dropwise to aceticanhydride in the reaction kettle; Carried out esterification 2 hours, washing, concentrated obtains d-alpha-tocopherol acetic ester bullion, this bullion and 450 gram anhydrous methanols, ethanol, Virahol mixed solution (volume ratio 2: 2: 1) is mixed again; Upper prop, control upper prop flow, temperature are 20～50 ℃, through the AB-8 absorption with macroporous adsorbent resin, effluent concentrates precipitation; Liquid concentrator mixes with 300 gram ethanol, 100 gram ETHYLE ACETATE and 50 gram propyl acetates again, adds 3 gram gacs, 1 gram silica gel and 1.5 gram atlapulgites, under 60 ℃ of temperature constant temperature; Adopt the outer circulation mode, circulated 2 hours, filter, concentrate; This liquid concentrator under the condition of high vacuum, carries out short-range molecular distillation and makes with extra care again, obtains d-alpha-tocopherol acetic ester finished product.Record d-alpha-tocopherol acetate content 98.2%; Specific rotatory power+24.1 °; Heavy metal (in Pb) 9.6ppm; Benzopyrene≤2ppb.
Need to prove inert organic solvents, polar solvent, catalyzer, polymeric adsorbent in the foregoing description in addition, remove agent, remove the coupling that agent dosage etc. can also have multiple combination.
Claims (2)
1. the preparation method of the highly purified d-alpha-tocopherol of a low benzopyrene acetic ester may further comprise the steps:
(A) the d-alpha-tocopherol is mixed with inert organic solvents, catalyzer in certain proportion; About 35 ℃ of controlled temperature, slowly aceticanhydride is added dropwise in the reaction kettle, carries out esterification about 2 hours; Reaction finishes water flush away catalyzer, concentrates then and obtains d-alpha-tocopherol acetic ester bullion; Described inert organic solvents is any in normal hexane, the sherwood oil; Described d-alpha-tocopherol and inert organic solvents blending ratio are 1: 3-5; Described catalyzer is any in zinc chloride, the aluminum chloride; Described catalyzer dosage is in d-alpha-tocopherol weight 3-5%;
(B) d-alpha-tocopherol acetic ester bullion is mixed with polar solvent according to a certain percentage; Upper prop, control upper prop flow, temperature are 20～50 ℃, through resin absorption; With weakly acidic organic impurity absorption, effluent obtains the higher d-alpha-tocopherol acetic ester bullion of purity after concentrating precipitation; Described polar solvent be in anhydrous methanol, ethanol, the Virahol any or plant arbitrarily and mix with arbitrary proportion; Described d-alpha-tocopherol acetic ester bullion and polar solvent blending ratio are 1: 3-5; Described upper prop flow is 1%～5% of a resin volume for the PM add-on; Described resin is any in D-101 type macroporous adsorbent resin, AB-8 type macroporous adsorbent resin, DA-201 type macroporous adsorbent resin, X-5 type macroporous adsorbent resin, DM130 macroporous adsorbent resin, the DM-301 type macroporous adsorbent resin;
(C) above-mentioned purity is higher d-alpha-tocopherol acetic ester bullion mixes with inert organic solvents, adds a certain proportion of agent that removes, and under 60 ℃ of temperature constant temperature, adopts the outer circulation mode, circulates 2 hours, filters to remove to remove agent, concentrates precipitation; Described inert organic solvents be in ethanol, methyl acetate, ETHYLE ACETATE, propyl acetate, butylacetate, the Virahol any or plant arbitrarily and mix with arbitrary proportion; Described d-alpha-tocopherol acetic ester bullion and inert organic solvents blending ratio are 1: 3-5; It is described that to remove agent be a kind of or any kind mix with arbitrary proportion in gac, silica gel, atlapulgite, the molecular sieve; The described agent dosage that removes is in d-alpha-tocopherol acetic ester bullion weight 4-6%;
(D) with the d-alpha-tocopherol acetic ester behind the above-mentioned concentrated precipitation under the condition of high vacuum, it is refining to carry out short-range molecular distillation, promptly obtains the low highly purified d-alpha-tocopherol of benzopyrene acetic ester finished product.
2. the preparation method of the highly purified d-alpha-tocopherol of a kind of low benzopyrene according to claim 1 acetic ester is characterized in that, described to remove agent be that gac, silica gel any or two kinds mix with arbitrary proportion.
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| CN104520285A (en) * | 2012-08-10 | 2015-04-15 | 帝斯曼知识产权资产管理有限公司 | Tocopherols with reduced content of phenolic impurities |
| CN104520283A (en) * | 2012-08-10 | 2015-04-15 | 帝斯曼知识产权资产管理有限公司 | Tocopherols with reduced content of dehydrotocopherol |
| CN105175384A (en) * | 2015-07-20 | 2015-12-23 | 宜春大海龟生命科学有限公司 | Method for removing polycyclic aromatic hydrocarbons from natural vitamin E |
| CN105801552A (en) * | 2016-05-19 | 2016-07-27 | 浙江伊宝馨生物科技股份有限公司 | Preparation method of high-purity natural d-alpha-tocopheryl acetate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104520285A (en) * | 2012-08-10 | 2015-04-15 | 帝斯曼知识产权资产管理有限公司 | Tocopherols with reduced content of phenolic impurities |
| CN104520283A (en) * | 2012-08-10 | 2015-04-15 | 帝斯曼知识产权资产管理有限公司 | Tocopherols with reduced content of dehydrotocopherol |
| CN105175384A (en) * | 2015-07-20 | 2015-12-23 | 宜春大海龟生命科学有限公司 | Method for removing polycyclic aromatic hydrocarbons from natural vitamin E |
| CN105801552A (en) * | 2016-05-19 | 2016-07-27 | 浙江伊宝馨生物科技股份有限公司 | Preparation method of high-purity natural d-alpha-tocopheryl acetate |
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