CN102584769B - Preparation method of natural VE with content of more than 99% - Google Patents
Preparation method of natural VE with content of more than 99% Download PDFInfo
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- CN102584769B CN102584769B CN 201110428798 CN201110428798A CN102584769B CN 102584769 B CN102584769 B CN 102584769B CN 201110428798 CN201110428798 CN 201110428798 CN 201110428798 A CN201110428798 A CN 201110428798A CN 102584769 B CN102584769 B CN 102584769B
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Abstract
The invention discloses a preparation method of natural VE (vitamin E) with the content of more than 99%. Natural VE with the content of 40% is adopted, is dissolved according to a certain ratio in ethanol with the content of 99%, is cooled to be about 15 DEG C, and is filtered to remove undissolved substances of ethanol; a secondary absorption manner is adopted, big hole absorbing resin is used for absorbing acid impurities, pigment and the like, effluent liquid is absorbed by anion strongly basic resin to absorb natural VE, then anion strongly basic resin is washed by ethanol with the content of 99% to remove impurities that do not absorb methyl ester and the like, next a release agent is used for releasing VE, and eluate is in low temperature crystallization to be a certain temperature, and is filtered through micro holes to remove undissolved substances of ethanol; a special removal agent is added to remove polycyclic aromatic hydrocarbons (PAH) and absorb other impurities, after the removal agent is removed through filtering, concentration and exsolution are conducted, and finally the natural vitamin E is refined through three-grade molecules distillation. The content, the purity and the like of the product obtained through the invention can meet the quality requirement of European Union member countries.
Description
Technical field
The present invention relates to the natural additive for foodstuff production technical field, be specifically related to a kind of preparation method of content 99% above natural VE.
Background technology
Vitamin-E (being called for short VE) has important physiological function, is the essential nutrient substance of humans and animals, is widely used in the industries such as medicine, healthcare products, cosmetics and skincare product, food and feed additive.At present become demand and the fastest VITAMIN kind of sale growth on the world market, compared with synthetic VE, natural VE with its high reactivity, pure natural and the characteristic such as safe and reliable, more is subject to people's favor again.Western countries' natural VE industry starting early, on manufacturing technology and product technology level, all lead over domestic enterprise at present, but owing to be subjected to the restriction of raw material resources (edible vegetable oil deodorization distillate), the growth of demand often is unable to catch up with in the growth of the national output such as America and Europe, need to remedy market has openings by import, but American-European countries is very harsh to the requirement of natural VE, and content, purity, trace impurity etc. are had strict quality index requirement.In order to meet the need of market, research and develop a kind of preparation method of content 99% above natural VE.
Summary of the invention
The technical problem to be solved in the present invention provides the preparation method that content, purity of a kind of products obtained therefrom etc. can satisfy the content 99% above natural VE of European Union member countries' specification of quality.
For achieving the above object, technical scheme of the present invention is:
Adopt 40% natural VE (plant oil deodorizing distillates such as available soybean, vegetable seed or corn extract and make), carry out first pre-treatment, dissolve with certain proportion with 99% ethanol, be cooled to about 15 ℃, remove by filter alcohol-insoluble substance; Adopt secondary absorption again, use first absorption with macroporous adsorbent resin acidic impurities and pigment etc., effluent liquid is used 99% washing with alcohol negatively charged ion strong alkali resin again with negatively charged ion strong alkali resin absorption natural VE, removes impurity such as not adsorbing methyl esters; Then free VE with release agent, the elutriant cold analysis through millipore filtration, is removed alcohol-insoluble substance to certain temperature; Add and specifically to remove agent and remove polynuclear aromatics and adsorb other impurity, remove by filter remove agent after, concentrated, precipitation, refining and get final product finally by three grades of molecules distillations.
The preparation method of content 99% above natural VE may further comprise the steps:
(A) 40% natural VE and 99% ethanol are prepared fully dissolving by 1: 5 weight ratio, be cooled to about 15 ℃, remove by filter alcohol-insoluble substance, treat upper prop; Described 40% natural VE weight ratio consists of and comprises d-alpha-tocopherol 4-12%, β+gama tocopherol 18-32%, methyltocol 4-10% (all the other are same);
(B) upper prop absorption: adopt secondary absorption, first step ion column absorption with macroporous adsorbent resin is removed acidic impurities and pigment etc., and effluent liquid with the absorption of negatively charged ion strong alkali resin, adsorbs natural VE through second stage ion column; Described macroporous adsorbent resin is D-101 type macroporous adsorbent resin or AB-8 type macroporous adsorbent resin or DM130 macroporous adsorbent resin; Described negatively charged ion highly basic polymeric adsorbent is HZ202 type strong base anion resins or D204 type strong base anion resins;
(C) with 99% washing with alcohol second stage ion column, remove impurity such as not adsorbing methyl esters;
(D) use CO
2, acetic acid frees VE, resin is regenerated with potassium hydroxide-ethanol solution after freeing, and gets batch absorption ready and uses;
(E) elutriant is through continuously cold analysis, and temperature is controlled about 8 ℃, and micropore (0.5 μ) filters, and further removes alcohol-insoluble substance;
(F) above-mentioned filtrate adding certain proportion specifically removes agent, under 60 ℃ of temperature constant temperature, adopts the outer circulation mode, circulates 2 hours, filters to remove to remove agent; It is described that specifically to remove agent be that any or two kinds mix with arbitrary proportion in gac, the silica gel; The described agent dosage that removes is with VE weighing scale 4-6%;
(G) concentrated, precipitation obtains the natural VE more than 95%;
(H) concentrated, precipitation liquid distills through three grades of molecules, about 150 ℃ of one-level control temperature are removed lower boiling light component substance, about 180 ℃ of secondary control temperature, control about 230 ℃ of temperature, further remove high boiling substance and namely get content 99% above finished product for three grades.
The preparation method of a kind of content 99% above natural VE of the present invention, products obtained therefrom content is high, natural VE content 〉=99%, color and luster≤8Gardner, polynuclear aromatics (PAHs) content＜25ppb (1ppb is part per billion), lightweight part＜20ppb wherein, heavy part＜5ppb, benzopyrene＜2ppb in the heavy part.
Embodiment
The present invention is further illustrated below in conjunction with embodiment, and following each embodiment only is used for explanation the present invention, but to the present invention without limits.
Embodiment one
Get 40% natural VE 200g, add 99% ethanol 1000g, dissolving is cooled to about 15 ℃, filters; Filtrate is through being equipped with the first step ion column absorption of AB-8 type macroporous adsorbent resin, again through the second stage ion column absorption of HZ202 type strong base anion resins is housed, with 99% washing with alcohol second stage ion column; Free VE with CO2, acetic acid, resin is regenerated with potassium hydroxide-ethanol solution after freeing, and to about 8 ℃ of temperature controls, micropore (0.5 μ) filters elutriant through continuous cold analysis; Filtrate adds the 10g gac, controls under 60 ℃ of constant temperature, adopts the outer circulation mode, circulates 2 hours, filters, concentrated precipitation; Through three grades of molecule distillations, one-level is controlled about 150 ℃ of temperature again, and about 180 ℃ of secondary control temperature are controlled about 230 ℃ of temperature for three grades and got product.Described 40% natural VE weight ratio consists of and comprises d-alpha-tocopherol 4-12%, β+gama tocopherol 18-32%, methyltocol 4-10% (together lower).Natural VE content 99.1% after testing, color and luster≤8Gardner, polynuclear aromatics (PAHs) content 23ppb; Lightweight part 18ppb wherein, heavy part 4ppb, benzopyrene＜2ppb in the heavy part.
Embodiment two
Get 40% natural VE 200g, add 99% ethanol 1000g, dissolving is cooled to about 15 ℃, filters; Filtrate is through being equipped with the first step ion column absorption of D-101 type macroporous adsorbent resin, again through the second stage ion column absorption of HZ202 type strong base anion resins is housed, with 99% washing with alcohol second stage ion column; Free VE with CO2, acetic acid, resin is regenerated with potassium hydroxide-ethanol solution after freeing, and to about 8 ℃ of temperature controls, micropore (0.5 μ) filters elutriant through continuous cold analysis; Filtrate adds the 10g gac, controls under 60 ℃ of constant temperature, adopts the outer circulation mode, circulates 2 hours, filters, concentrated precipitation; Through three grades of molecule distillations, one-level is controlled about 150 ℃ of temperature again, and about 180 ℃ of secondary control temperature are controlled about 230 ℃ of temperature for three grades and got product.Natural VE content 99.2% after testing, color and luster≤8Gardner, polynuclear aromatics (PAHs) content 24ppb; Lightweight part 19ppb wherein, heavy part 4ppb, benzopyrene＜2ppb in the heavy part.
Embodiment three
Get 40% natural VE 200g, add 99% ethanol 1000g, dissolving is cooled to about 15 ℃, filters; Filtrate is through being equipped with the first step ion column absorption of AB-8 type macroporous adsorbent resin, again through the second stage ion column absorption of D204 type strong base anion resins is housed, with 99% washing with alcohol second stage ion column; Free VE with CO2, acetic acid, resin is regenerated with potassium hydroxide-ethanol solution after freeing, and to about 8 ℃ of temperature controls, micropore (0.5 μ) filters elutriant through continuous cold analysis; Filtrate adds the 8g gac, controls under 60 ℃ of constant temperature, adopts the outer circulation mode, circulates 2 hours, filters, concentrated precipitation; Through three grades of molecule distillations, one-level is controlled about 150 ℃ of temperature again, and about 180 ℃ of secondary control temperature are controlled about 230 ℃ of temperature for three grades and got product.Natural VE content 99.3% after testing, color and luster≤8Gardner, polynuclear aromatics (PAHs) content 20ppb; Lightweight part 18ppb wherein, heavy part 4.8ppb, benzopyrene＜2ppb in the heavy part.
Embodiment four
Get 40% natural VE 200g, add 99% ethanol 1000g, dissolving is cooled to about 15 ℃, filters; Filtrate is through being equipped with the first step ion column absorption of D-101 type macroporous adsorbent resin, again through the second stage ion column absorption of D204 type strong base anion resins is housed, with 99% washing with alcohol second stage ion column; Free VE with CO2, acetic acid, resin is regenerated with potassium hydroxide-ethanol solution after freeing, and to about 8 ℃ of temperature controls, micropore (0.5 μ) filters elutriant through continuous cold analysis; Filtrate adds 12g silica gel, controls under 60 ℃ of constant temperature, adopts the outer circulation mode, circulates 2 hours, filters, concentrated precipitation; Through three grades of molecule distillations, one-level is controlled about 150 ℃ of temperature again, and about 180 ℃ of secondary control temperature are controlled about 230 ℃ of temperature for three grades and got product.Natural VE content 99.2% after testing, color and luster≤8Gardner, polynuclear aromatics (PAHs) content 21ppb; Lightweight part 17ppb wherein, heavy part 4.5ppb, benzopyrene＜2ppb in the heavy part.
Embodiment five
Get 40% natural VE 150g, add 99% ethanol 750g, dissolving is cooled to about 15 ℃, filters; Filtrate is through being equipped with the first step ion column absorption of DM130 type macroporous adsorbent resin, again through the second stage ion column absorption of HZ202 type strong base anion resins is housed, with 99% washing with alcohol second stage ion column; Free VE with CO2, acetic acid, resin is regenerated with potassium hydroxide-ethanol solution after freeing, and to about 8 ℃ of temperature controls, micropore (0.5 μ) filters elutriant through continuous cold analysis; Filtrate adds 6g gac and 3g silica gel, controls under 60 ℃ of constant temperature, adopts the outer circulation mode, circulates 2 hours, filters, concentrated precipitation; Through three grades of molecule distillations, one-level is controlled about 150 ℃ of temperature again, and about 180 ℃ of secondary control temperature are controlled about 230 ℃ of temperature for three grades and got product.Natural VE content 99.2% after testing, color and luster≤8Gardner, polynuclear aromatics (PAHs) content 21ppb; Lightweight part 17ppb wherein, heavy part 4.5ppb, benzopyrene＜2ppb in the heavy part.
Embodiment six
Get 40% natural VE 150g, add 99% ethanol 750g, dissolving is cooled to about 15 ℃, filters; Filtrate is through being equipped with the first step ion column absorption of AB-8 type macroporous adsorbent resin, again through the second stage ion column absorption of HZ202 type strong base anion resins is housed, with 99% washing with alcohol second stage ion column; Free VE with CO2, acetic acid, resin is regenerated with potassium hydroxide-ethanol solution after freeing, and to about 8 ℃ of temperature controls, micropore (0.5 μ) filters elutriant through continuous cold analysis; Filtrate adds 8g gac and 1g silica gel, controls under 60 ℃ of constant temperature, adopts the outer circulation mode, circulates 2 hours, filters, concentrated precipitation; Through three grades of molecule distillations, one-level is controlled about 150 ℃ of temperature again, and about 180 ℃ of secondary control temperature are controlled about 230 ℃ of temperature for three grades and got product.Natural VE content 99.1% after testing, color and luster≤8Gardner, polynuclear aromatics (PAHs) content 24ppb; Lightweight part 17ppb wherein, heavy part 4.2ppb, benzopyrene＜2ppb in the heavy part.
Embodiment seven
Get 40% natural VE 100g, add 99% ethanol 500g, dissolving is cooled to about 15 ℃, filters; Filtrate is through being equipped with the first step ion column absorption of D-101 type macroporous adsorbent resin, again through the second stage ion column absorption of HZ202 type strong base anion resins is housed, with 99% washing with alcohol second stage ion column; Free VE with CO2, acetic acid, resin is regenerated with potassium hydroxide-ethanol solution after freeing, and to about 8 ℃ of temperature controls, micropore (0.5 μ) filters elutriant through continuous cold analysis; Filtrate adds 3g gac and 3g silica gel, controls under 60 ℃ of constant temperature, adopts the outer circulation mode, circulates 2 hours, filters, concentrated precipitation; Through three grades of molecule distillations, one-level is controlled about 150 ℃ of temperature again, and about 180 ℃ of secondary control temperature are controlled about 230 ℃ of temperature for three grades and got product.Natural VE content 99.1% after testing, color and luster≤8Gardner, polynuclear aromatics (PAHs) content 23ppb; Lightweight part 19ppb wherein, heavy part 4.5ppb, benzopyrene＜2ppb in the heavy part.
Embodiment eight
Get 40% natural VE 100g, add 99% ethanol 500g, dissolving is cooled to about 15 ℃, filters; Filtrate is through being equipped with the first step ion column absorption of D-101 type macroporous adsorbent resin, again through the second stage ion column absorption of D204 type strong base anion resins is housed, with 99% washing with alcohol second stage ion column; Free VE with CO2, acetic acid, resin is regenerated with potassium hydroxide-ethanol solution after freeing, and to about 8 ℃ of temperature controls, micropore (0.5 μ) filters elutriant through continuous cold analysis; Filtrate adds 3g gac and 2g silica gel, controls under 60 ℃ of constant temperature, adopts the outer circulation mode, circulates 2 hours, filters, concentrated precipitation; Through three grades of molecule distillations, one-level is controlled about 150 ℃ of temperature again, and about 180 ℃ of secondary control temperature are controlled about 230 ℃ of temperature for three grades and got product.Natural VE content 99.2% after testing, color and luster≤8Gardner, polynuclear aromatics (PAHs) content 20ppb; Lightweight part 18ppb wherein, heavy part 4.1ppb, benzopyrene＜2ppb in the heavy part.
Claims (2)
1. the preparation method of content 99% an above natural VE is characterized in that, may further comprise the steps:
(A) 40% natural VE and 99% ethanol are pressed fully dissolving of 1:5 weight ratio preparation, be cooled to about 15 ℃, filter;
(B) upper prop absorption: adopt secondary absorption, first step ion column absorption with macroporous adsorbent resin is removed acidic impurities and pigment etc., and effluent liquid with the absorption of negatively charged ion strong alkali resin, adsorbs natural VE through second stage ion column; Described macroporous adsorbent resin is D-101 type macroporous adsorbent resin or AB-8 type macroporous adsorbent resin or DM130 macroporous adsorbent resin; Described negatively charged ion highly basic polymeric adsorbent is HZ202 type strong base anion resins or D204 type strong base anion resins;
(C) with 99% washing with alcohol second stage ion column;
(D) free VE with CO2, acetic acid, resin is regenerated with potassium hydroxide-ethanol solution after freeing;
(E) elutriant is through continuously cold analysis, and temperature is controlled about 8 ℃, 0.5 μ m millipore filtration;
(F) above-mentioned filtrate adding certain proportion specifically removes agent, under 60 ℃ of temperature constant temperature, adopts the outer circulation mode, circulates 2 hours, filters; It is described that specifically to remove agent be that any or two kinds mix with arbitrary proportion in gac, the silica gel; The described agent dosage that removes is with VE weighing scale 4-6%;
(G) concentrated, precipitation;
(H) concentrated, precipitation liquid distills through three grades of molecules, about 150 ℃ of one-level control temperature, and about 180 ℃ of secondary control temperature are controlled about 230 ℃ of temperature for three grades and are got product.
2. the preparation method of a kind of content 99% above natural VE according to claim 1 is characterized in that, described 40% natural VE weight ratio consists of and comprises d-alpha-tocopherol 4-12%, β+gama tocopherol 18-32%, methyltocol 4-10%.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103304533A (en) * | 2013-06-13 | 2013-09-18 | 宁波大红鹰生物工程股份有限公司 | Method for removing dioxin in natural vitamin E |
| CN104230872B (en) * | 2014-09-05 | 2016-09-07 | 宁波大红鹰生物工程股份有限公司 | A kind of process for separation and purification of d-Delta-Tocopherol |
| 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 |
| CN104829582B (en) * | 2015-05-05 | 2017-05-17 | 陕西源邦生物技术有限公司 | Method for extracting high content natural vitamin E from annatto |
| CN104961718B (en) * | 2015-07-07 | 2017-03-08 | 浙江伊宝馨生物科技股份有限公司 | The special equipment of micro objectionable impurities 6-(10-hydroxy-6-oxo-trans-1-undecenyl)-.beta.-resorcylic acid lactone and removal methods in natural Vitamin E |
| CN107903236B (en) * | 2017-11-24 | 2021-05-25 | 宁波大红鹰生物工程股份有限公司 | Method for removing mineral oil in natural vitamin E |
| CN112920152A (en) * | 2019-12-06 | 2021-06-08 | 中国科学院大连化学物理研究所 | High-efficiency preparation chromatographic method for removing zearalenone from natural vitamin E |
| CN111233813A (en) * | 2020-03-05 | 2020-06-05 | 浙江伊宝馨生物科技股份有限公司 | Method for removing glycidyl ester in mixed tocopherol |
| CN111269209A (en) * | 2020-03-21 | 2020-06-12 | 浙江伊宝馨生物科技股份有限公司 | Method for removing mineral oil in VE |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401644A (en) * | 2002-09-19 | 2003-03-12 | 浙江大学 | Process for extracting high content mixed tocopherol |
| CN101643467A (en) * | 2009-09-14 | 2010-02-10 | 天津大学 | Method for extracting vitamin E and phytosterin from cottonseed oil deodorizer distillate |
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| JP5700188B2 (en) * | 2008-02-13 | 2015-04-15 | 国立大学法人東北大学 | Method for simultaneous production of tocotrienol and biodiesel fuel from fats and oils |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401644A (en) * | 2002-09-19 | 2003-03-12 | 浙江大学 | Process for extracting high content mixed tocopherol |
| CN101643467A (en) * | 2009-09-14 | 2010-02-10 | 天津大学 | Method for extracting vitamin E and phytosterin from cottonseed oil deodorizer distillate |
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| JP特开2009-190989A 2009.08.27 |
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