CN103304533A - Method for removing dioxin in natural vitamin E - Google Patents
Method for removing dioxin in natural vitamin E Download PDFInfo
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- CN103304533A CN103304533A CN2013102344786A CN201310234478A CN103304533A CN 103304533 A CN103304533 A CN 103304533A CN 2013102344786 A CN2013102344786 A CN 2013102344786A CN 201310234478 A CN201310234478 A CN 201310234478A CN 103304533 A CN103304533 A CN 103304533A
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Abstract
The invention provides a method for removing dioxin in natural vitamin E. The method comprises the following steps of: taking the natural vitamin E as a solute, taking an inert organic solvent as a solvent, adding a removal agent accounting for 5-10% by weight of the natural vitamin E, controlling the temperature to be 55-60 DEG C under nitrogen protection, filtering and concentrating after full mixing, and further refining by molecular distillation. By adopting the method for removing the dioxin in the natural vitamin E, provided by the invention, the dioxin component in the natural vitamin E can be effectively removed, the total content of the dioxin is less than 0.75pg/g (one trillionth), and the total amount of dioxin-like substances and the dioxin is less than 1.25pg/g, which is lower than the European standard; and simultaneously, the operation process is simple, the cost is low, the environmental pollution is little, and harmful substances in the natural vitamin E can be effectively removed.
Description
Technical field
The present invention relates to the natural VE production field, relate in particular to a kind of method that removes natural VE Zhong dioxin.
Background technology
Dioxin (Dioxin), claim two oxa-glutinous rehmannias again, be that the serious lipid-soluble substance dioxin of a kind of colorless and odorless, toxicity is actually abbreviation of dioxin (Dioxins), what it referred to is not a kind of one matter, but structure and character very similar two big class organic compound that comprise numerous congeners or isomer all.Dioxin comprises 210 kinds of compounds, and this class material is highly stable, and fusing point is higher, and the utmost point is insoluble in water, can be dissolved in most of organic solvent, is the lipid-soluble substance of colorless and odorless, thus be very easy to accumulation in vivo, serious to human body harm.
Dioxin has the characteristic that is similar to " 12 big hazardous material ", and " 12 big hazardous material " is one group of dangerous chemicals that is called as persistence organic pollutant.Experimental results show that dioxin can damage multiple organ and system, in case enter human body, will be resident for a long time, because itself have chemical stability and be easy to be absorbed by fatty tissue, and from then on long-term savings may see through indirect physiological pathway and carcinogenic in vivo.Their transformation period in vivo are estimated as 7 to 11 years.The ， dioxin accumulates in the food chain easily in environment.The degree that the more high ， dioxin of degree of dependence animal-derived food product is built up in the food chain is just more high.
European Union's rules and regulations, the content of total dioxin is less than 0.75pg/g(1/100000000000th), the total amount of class dioxin and dioxin is less than 1.25pg/g.Because dioxin is very micro-in natural VE, it also is very difficult removing, and does not have as yet in the same industry at present to meet industrial production and have the removal methods of using value economically.How to remove the micro-dioxin in the natural VE, become a worth problem demanding prompt solution.
Summary of the invention
Present situation at not occurring removing the method for micro-dioxin in the natural VE in the prior art as yet the invention provides a kind of removal methods.
The invention provides a kind of method that removes natural VE Zhong dioxin, may further comprise the steps:
1) with natural VE and the inert solvent mixed with weight ratio 1:1-6, add in natural VE weight 5-10% remove agent after, add nitrogen, be heated to 55-60 ℃, keep temperature, and fully mix;
2) filter through well-beaten mixing solutions, after the collection filtrate filtrate is concentrated;
3) collect concentrated solution and concentrated solution carried out molecular distillation, obtain removing the natural VE of dioxin.
Preferably, removing inert solvent in the method for natural VE Zhong dioxin is at least a in methyl alcohol, ethanol, ethyl acetate, normal hexane, acetone, the butanone;
Preferably, the inert solvent that removes in the method for natural VE Zhong dioxin is ethanol or ethyl acetate;
Preferably, the agent that removes that removes in the method for natural VE Zhong dioxin is at least a in gac, atlapulgite, diatomite, the silica gel;
Preferably, the agent that removes that removes in the method for natural VE Zhong dioxin is gac or atlapulgite;
Preferably, remove the method steps 2 of natural VE Zhong dioxin) in filtrate concentrate to adopt scraper evaporator to steam except concentrating.
Adopt the method that removes natural VE Zhong dioxin of the present invention, can effectively remove De dioxin composition in the natural VE, technology is simple, cost is low, environmental pollution is little, handle the content of the total dioxin in back less than 0.75pg/g(1/100000000000th), the total amount of class dioxin and dioxin is less than 1.25pg/g.
Embodiment
In order more to be expressly understood technology contents of the present invention, below embodiments of the present invention are described in further detail.
Be solute with the natural VE, at least a as solvent with in inert organic solvents methyl alcohol, ethanol, ethyl acetate, normal hexane, acetone, the butanone, inert organic solvents preferred alcohol or ethyl acetate, ratio according to weight ratio 1:1-6 is mixed in reactor, add then and remove at least a of agent gac, atlapulgite, diatomite, silica gel, preferred gac or atlapulgite in natural VE weight 5-10%.Feed nitrogen, oxygen in the replacement reaction kettle is exposed to deterioration by oxidation in the air to prevent vitamin-E.Under nitrogen protection, 55 ℃-60 ℃ of control reactor temperatures after fully mixing, filter, and utilize scraper evaporator to steam except unnecessary solvent, and concentrated filtrate then gets final product with molecular distillation is refining.
Embodiment 1
Get natural VE 100g, be dissolved in the 200g ethanol, add the 5g gac, under the nitrogen protection, be heated to 55 ℃, stirred 3 hours, stop after-filtration, behind the filtrate steaming removal solvent, obtain product through molecular distillation again.， dioxin content 0.42pg/g ， dioxin and Lei dioxin total amount 0.93pg/g after testing.
Embodiment 2
Get natural VE 100g, be dissolved in the 300g ethyl acetate, add the 10g gac, under the nitrogen protection, be heated to 60 ℃, stirred 3 hours, stop after-filtration, behind the filtrate steaming removal solvent, obtain product through molecular distillation again.， dioxin content 0.59pg/g ， dioxin and Lei dioxin total amount 0.96pg/g after testing.
Embodiment 3
Get natural VE 100g, be dissolved in the 600g ethyl acetate, add the 8g gac, under the nitrogen protection, be heated to 58 ℃, stirred 2 hours, stop after-filtration, behind the filtrate steaming removal solvent, obtain product through molecular distillation again.， dioxin content 0.55pg/g ， dioxin and Lei dioxin total amount 0.87pg/g after testing.
Embodiment 4
Get natural VE 100g, be dissolved in the 500g ethanol, add the 9g gac, under the nitrogen protection, be heated to 56 ℃, stirred 4 hours, stop after-filtration, behind the filtrate steaming removal solvent, obtain product through molecular distillation again.， dioxin content 0.31pg/g ， dioxin and Lei dioxin total amount 0.72pg/g after testing.
Embodiment 5
Get natural VE 100g, be dissolved in the 100g normal hexane, add the 6g gac, under the nitrogen protection, be heated to 60 ℃, stirred 4 hours, stop after-filtration, behind the filtrate steaming removal solvent, obtain product through molecular distillation again.， dioxin content 0.64pg/g ， dioxin and Lei dioxin total amount 1.10pg/g after testing.
Embodiment 6
Get natural VE 100g, be dissolved in the 300g butanone, add the 5g gac, under the nitrogen protection, be heated to 60 ℃, stirred 5 hours, stop after-filtration, behind the filtrate steaming removal solvent, obtain product through molecular distillation again.， dioxin content 0.71pg/g ， dioxin and Lei dioxin total amount 1.01pg/g after testing.
Adopt the present invention to remove the method for natural VE Zhong dioxin, but De dioxin composition in the effective elimination natural VE, make the content of total dioxin less than 0.75pg/g(1/100000000000th); the total amount of class dioxin and dioxin is lower than European Union's standard, simultaneously less than 1.25pg/g, operating procedure is simple, cost is low, and environmental pollution is little, is the method for objectionable impurities in the effective removal natural VE.
The specific embodiment of the present invention has above been described.But those of ordinary skill in the art can be understood, and under the situation without departing from the spirit and scope of the present invention, can also do various changes and replacement to the specific embodiment of the present invention.These changes and replacement all drop in claims restricted portion of the present invention.
Claims (6)
1. a method that removes dioxin in the natural VE is characterized in that, described removal methods may further comprise the steps:
1) with natural VE and the inert solvent mixed with weight ratio 1:1-6, add in natural VE weight 5-10% remove agent after, add nitrogen, be heated to 55-60 ℃, keep temperature, and fully mix;
2) filtration is described through well-beaten mixing solutions, after the collection filtrate described filtrate is concentrated;
3) collect concentrated solution and described concentrated solution carried out molecular distillation, obtain removing the natural VE of dioxin.
2. the method that removes natural VE Zhong dioxin as claimed in claim 1 is characterized in that, described inert solvent is at least a in methyl alcohol, ethanol, ethyl acetate, normal hexane, acetone, the butanone.
3. the method that removes natural VE Zhong dioxin as claimed in claim 2 is characterized in that, described inert solvent is ethanol or ethyl acetate.
4. the method that removes natural VE Zhong dioxin as claimed in claim 1 is characterized in that, described to remove agent be at least a in gac, atlapulgite, diatomite, the silica gel.
5. the method that removes natural VE Zhong dioxin as claimed in claim 4 is characterized in that, described to remove agent be gac or atlapulgite.
6. the method that removes natural VE Zhong dioxin as claimed in claim 1 is characterized in that, described step 2) in filtrate concentrate to adopt scraper evaporator to steam except concentrating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013102344786A CN103304533A (en) | 2013-06-13 | 2013-06-13 | Method for removing dioxin in natural vitamin E |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013102344786A CN103304533A (en) | 2013-06-13 | 2013-06-13 | Method for removing dioxin in natural vitamin E |
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| CN103304533A true CN103304533A (en) | 2013-09-18 |
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| CN2013102344786A Pending CN103304533A (en) | 2013-06-13 | 2013-06-13 | Method for removing dioxin in natural vitamin E |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103630439A (en) * | 2013-11-27 | 2014-03-12 | 中国检验检疫科学研究院 | Rapid precleaning method for detecting dioxins |
| CN105585552B (en) * | 2014-11-13 | 2018-06-26 | 丰益(上海)生物技术研发中心有限公司 | A kind of decoloration purification process of vitamin E |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317365A (en) * | 2000-02-14 | 2001-10-17 | 三浦工业株式会社 | Adsorption material for dioxine |
| CN1844117A (en) * | 2006-03-10 | 2006-10-11 | 浙江华源制药科技开发有限公司 | Method for removing micro polynary arene in natural vitamine E |
| CN102584769A (en) * | 2011-12-20 | 2012-07-18 | 浙江华源制药科技开发有限公司 | Preparation method of natural VE with content of more than 99% |
-
2013
- 2013-06-13 CN CN2013102344786A patent/CN103304533A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317365A (en) * | 2000-02-14 | 2001-10-17 | 三浦工业株式会社 | Adsorption material for dioxine |
| CN1844117A (en) * | 2006-03-10 | 2006-10-11 | 浙江华源制药科技开发有限公司 | Method for removing micro polynary arene in natural vitamine E |
| CN102584769A (en) * | 2011-12-20 | 2012-07-18 | 浙江华源制药科技开发有限公司 | Preparation method of natural VE with content of more than 99% |
Non-Patent Citations (1)
| Title |
|---|
| MARY KIM HALBERT ET AL.: "Dioxin and furan contamination of deodorizer distillates and natural vitamin E supplements", 《JOURNAL OF FOOD COMPOSITION AND ANALYSIS》, vol. 20, 31 December 2007 (2007-12-31), pages 506 - 514, XP022106996, DOI: doi:10.1016/j.jfca.2007.02.001 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103630439A (en) * | 2013-11-27 | 2014-03-12 | 中国检验检疫科学研究院 | Rapid precleaning method for detecting dioxins |
| CN105585552B (en) * | 2014-11-13 | 2018-06-26 | 丰益(上海)生物技术研发中心有限公司 | A kind of decoloration purification process of vitamin E |
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Application publication date: 20130918 |