CN105585552B - A kind of decoloration purification process of vitamin E - Google Patents
A kind of decoloration purification process of vitamin E Download PDFInfo
- Publication number
- CN105585552B CN105585552B CN201410640346.8A CN201410640346A CN105585552B CN 105585552 B CN105585552 B CN 105585552B CN 201410640346 A CN201410640346 A CN 201410640346A CN 105585552 B CN105585552 B CN 105585552B
- Authority
- CN
- China
- Prior art keywords
- vitamin
- decoloration
- tocopherol
- product
- sample
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Pyrane Compounds (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The present invention provides a kind of decoloration purification process of vitamin E, the described method comprises the following steps：(a) composite decoloring agent is provided, decolorization is carried out to vitamin E product；(b) the vitamin E product after the decoloration as obtained by column chromatography eluent step (a) collects eluent flow point；(c) the eluent flow point of gained in step (b) is concentrated, the vitamin E for obtaining decolourizing after purification, wherein, in step (a), the composite decoloring agent is atlapulgite:Activated carbon:Diatomite:Magnesium silicate=100:50~100:30~70:10~50, by mass.The decoloration purification process of the vitamin E of the present invention can make the lighter of vitamin E, and viscosity reduces, and improves mobility, and can be improved the purity of vitamin E, and be lost less in purification process of decolourizing, and the rate of recovery of vitamin E is high.
Description
Technical field
The present invention relates to a kind of decoloration purification process of vitamin E.
Background technology
Vitamin E also known as tocopherol are a kind of fat-soluble vitamin, it is organic molten to be soluble in ethyl alcohol, acetone, n-hexane etc.
Agent has good antioxidation.Vitamin E is divided into natural VE and synthesising complex E, and natural VE generally contains
Have eight kinds of homologues, respectively alpha-tocopherol, alpha-tocotrienol, betatocopherol, β-tocotrienols, Gamma-Tocopherol, γ-
The bioactivity of tocotrienols, Delta-Tocopherol and δ-tocotrienols, wherein alpha-tocopherol is maximum, as drug and health products
Effect is preferable；The antioxidant activity of Delta-Tocopherol is most strong, especially suitable for being used as antioxidant in food, cosmetics.Natural dimension life
Plain E has a dextrorotation photolytic activity, and synthesising complex E is then the racemic modification that various optical isomers are formed, no optical activity.
Vitamin E is nutrient needed by human, has important physiological function, is widely used in food, health products, change
The industries such as cosmetic, medicine, feed.Natural VE is industrially prepared mainly using the deodorization distillate of vegetable oil as original at present
Material, by esterification, varies with temperature the characteristics of changes in solubility is larger, through cold analysis using phytosterol in fatty acid methyl ester
Phytosterol is crystallized and be filtered to remove, then fatty acid methyl ester is removed with vacuum distillation, most afterwards through molecular distillation or supercritical extract
Obtain the concentrated product for the vitamin E that total tocopherol content is about 50%.The concentrated product, can through adsorption and desorption by resin, purifying
It is 90% and above vitamin E to obtain content, which through hydroxymethylation, can turn other tocopherol homologues again
Turn to the higher alpha-tocopherol of bioactivity.Vitamin E is golden yellow or flaxen sticky oil substance, due to producing work
The difference of skill in process of production, usually can remain or generate some coloured and colourless impurity in product, and cause color compared with
Depth, viscosity are larger, purity declines, and are unfavorable for the production of later product.Simultaneously as vitamin E is easily aoxidized, in air and light
It can slowly be aoxidized according under the conditions of and make color burn, purity reduces, so as to influence its appearance and use.
For the decoloration impurities removal of vitamin E, current correlative study is simultaneously few, and that is reported substantially utilizes activity
Charcoal or atlapulgite carry out adsorption bleaching.For example, in Chinese patent application CN101921254B, using activated carbon and activity
Carclazyte is with 1:2~1:3 ratio mixing, to decolourize to vitamin E product.In Chinese patent application CN 102382095A
In, decoloration removal of impurities is carried out to alpha-tocopherol using macroreticular resin.In addition, also some documents are used in refined vitamin E product
The fillers such as silica gel carry out column chromatography processing.For above-mentioned discoloration method, although there is certain decolorizing effect, there are still some
It is insufficient：It is handled according to activated carbon or atlapulgite, the color of product is shoaled, but product could not reduce viscosity and improvement
Mobility, and the purity of product is not obviously improved；It decolourizes according to purification on normal-phase silica gel for chromatography media, then it can be because
The loss that product generates suction-operated with silica gel and causes comparison high, and the regeneration of purification on normal-phase silica gel is also a problem；Macropore
Though resin treatment has certain decolorizing effect, purification effect is unsatisfactory.
For some practical problems present on, the present inventor analyzes impurity present in vitamin E and color
Situation is deepened, it is found that the impurity in vitamin E is mainly derived from dimer, some pigments, wax and the sterols object of tocopherol
Matter, the intensification of color are mainly some the self-polymerization objects generated after being aoxidized in itself due to vitamin E.According to these research knots
Fruit, the present invention are decolourized using composite decoloring agent, are then further purified using molecular sieving effect so that vitamin E product first
While decoloration, the viscosity of product can be also significantly decreased, improves mobility, and the purity of sample can be improved, simultaneously
The loss of entire decoloration purification process sample is seldom, and product recovery rate is high.
Invention content
The purpose of the present invention is to provide a kind of decoloration purification process of vitamin E, this method can make the face of vitamin E
Discoloration is shallow, viscosity reduces, and can be improved the purity of vitamin E, and loss of the product in purification process of decolourizing is very
Few, in a preferred approach, the vitamin E rate of recovery is more than 95%.
The present invention provides a kind of decoloration purification process of vitamin E, the described method comprises the following steps：
(a) composite decoloring agent is provided, decolorization is carried out to vitamin E product；
(b) as column chromatography and with the vitamin E product after the decoloration obtained by eluent step (a), collection is washed
De- liquid stream point；
(c) the eluent flow point of gained in step (b) is concentrated, the vitamin E for obtaining decolourizing after purification,
Wherein, in step (a), the composite decoloring agent is atlapulgite:Activated carbon:Diatomite:Magnesium silicate=100:
50~100:30~70:10~50, by mass.
In step (a), the vitamin E product contains alpha-tocopherol, alpha-tocotrienol, betatocopherol, β-fertility
Any one or a few in trienol, Gamma-Tocopherol, γ-tocotrienols, Delta-Tocopherol, δ-tocotrienols, it is total to give birth to
The content of phenol is more than 30%.
In step (a), the composite decoloring agent is atlapulgite:Activated carbon:Diatomite:Magnesium silicate=100:50~
70:40~60:25~35, by mass.
In step (a), the addition of the composite decoloring agent is the 10~50% of the vitamin E product quality, excellent
Select 20~40%.
In step (b), it is additionally included in and is produced with the vitamin E after the decoloration of gained in the eluent step (a)
Before product, column chromatography medium, stripping equilibria chromatographic column are impregnated using the eluant, eluent, is preferably further included institute in step (a)
Vitamin E product dissolving after the decoloration obtained.
In step (b), the column chromatography medium include be selected from by sephadex SephadexLH-20,
At least one of group of SephadexG-100, Sephacryl and Ago-Gel Sepharose compositions, preferably glucan
Gel SephadexLH-20.
In step (b), the eluant, eluent includes being selected from by chloroform, methanol, dichloromethane, isopropanol and absolute ethyl alcohol group
Into at least one of group, preferably include to be selected from by chloroform:Methanol=3:1~3:2nd, dichloromethane:Methanol=3:1~3:2、
Dichloromethane:Isopropanol=3:1~3:2nd, chloroform:Isopropanol=3:1~3:2 and any one of the group of absolute ethyl alcohol composition,
By volume.
According to another aspect of the present invention, the present invention provides a kind of according to the preparation of the decoloration purification process of foregoing vitamin E
Vitamin E product.
According to another aspect of the invention, the present invention provides a kind of vitamin E product, the color of the vitamin E product
Pool value is for 12 hereinafter, preferably 11 hereinafter, more preferably less than 10；And/or 25 DEG C of viscosity of the vitamin E product is
1.42Pas hereinafter, and 70 DEG C of viscosity is 0.0503Pas hereinafter, it is preferred that 25 DEG C of viscosity is 0.130~1.42Pas,
And 70 DEG C of viscosity is 0.0156~0.0503Pas, more preferable 25 DEG C of viscosity is 0.130~1.26Pas, and 70 DEG C
Viscosity is 0.0156~0.0456Pas, and most preferably 25 DEG C of viscosity is 0.130~0.855Pas, and 70 DEG C of viscosity is
0.0156~0.0302Pas.
According to another aspect of the invention, the present invention provides a kind of decolorising agent, and the decolorising agent is atlapulgite:Activity
Charcoal:Diatomite:Magnesium silicate=100:50~100:30~70:10~50, preferably 100:50~70:40~60:25~35, it presses
Quality meter.
In accordance with a further aspect of the present invention, the present invention provides decolourize what is purified according to above-mentioned decolorising agent for vitamin E
Purposes.
The decoloration purification process of vitamin E according to the present invention, the content of obtained vitamin E can improve 4~
48%；Color and luster becomes yellow from brownish red, and Gardner (color and luster) value is down to 10~11 by more than 14；Viscosity significantly reduces；Dimension life
The plain E rate of recovery is more than 95%.
Compared with existing vitamin E decolouring technology, advantage of the invention is that：
(1) relative to the discoloration method for using activated carbon, atlapulgite, macroreticular resin etc., method of the invention decoloration effect
Fruit is more obvious, while can significantly improve the content of vitamin E in sample.
(2) method of the invention can make vitamin E product colour shoal and significantly reduce the viscous of vitamin E product
Degree.
(3) relative to the absorption decoloring method of silica gel, method of the invention selects the absorption of pigment in vitamin E and impurity
Selecting property is stronger, and the loss of vitamin E is seldom in purification process of decolourizing, and the rate of recovery is even up to more than 95%.
(4) after the composite decoloring agent in the present invention after use is by organic solvent elution activation, more than 70% can be restored
Adsorption capacity, can reuse, and chromatography media sephadex and Ago-Gel make without processing is i.e. recyclable
With.
Specific embodiment
The present invention vitamin E product contain alpha-tocopherol, alpha-tocotrienol, betatocopherol, β-tocotrienols,
Any one or a few in Gamma-Tocopherol, γ-tocotrienols, Delta-Tocopherol, δ-tocotrienols, total tocopherol contains
Amount is more than 30%.
In the decoloration purification process of the vitamin E of the present invention, before decolorization is carried out to vitamin E product, make
It is dissolved with organic solvent such as absolute ethyl alcohol, more than 90% hydrous ethanol, n-hexane, normal heptane, petroleum ether or anhydrous ether
Vitamin E product, the addition of the organic solvent are 1~5 times of the vitamin E product quality.
In step (a), the composite decoloring agent is atlapulgite:Activated carbon:Diatomite:Magnesium silicate=100:50~
100:30~70:10~50, optimum ratio 100:50~70:40~60:25~35.By using answering for above-mentioned specific combination
Decolorising agent is closed, vitamin E product colour can be made to shoal, significantly reduce the viscosity of vitamin E.Using heretofore described compound
Decolorising agent decolourizes, with obvious effects better than the common decolorising agents such as activated carbon, atlapulgite are used alone, moreover, at this
In the ratio range of composite decoloring agent, decolorizing effect is preferable, and except the ratio range, even if using identical decolorising agent
Composition, decolorizing effect are also weaker.
The addition of the composite decoloring agent is 10~50%, preferably the 20~40% of the vitamin E product quality.It is de-
Toner addition and vitamin E product quality need to can be only achieved good decolorizing effect according to a certain percentage, if decolorising agent
The ratio of addition is less than 10%, then decolorizing effect is insufficient, and color declines unobvious；If decolorising agent addition is more than 50%,
Then adsorption bleaching effect increases unobvious, and sample adsorbance increases, and sample loss is caused to increase.
In the decoloration purification process of the vitamin E of the present invention, at a temperature of 30~80 DEG C, the vitamin E is produced
Pint 1~5h of color, preferably decolourize 2~4h.If bleaching temperature is less than 30 DEG C, decolorizing effect is incomplete；If bleaching temperature
More than 80 DEG C, then the decomposition of sample is likely to result in.When bleaching time is less than 1h, decolorizing effect is incomplete；In decoloring reaction
During for more than 5h, decolorizing effect is not further added by.
In the decoloration purification process of the vitamin E of the present invention, in taking off with the middle gained of the eluent step (a)
Before vitamin E product after color, column chromatography medium is impregnated using the eluant, eluent, the column chromatography medium impregnated after being swollen is adopted
It is fitted into chromatographic column with wet method, then balances chromatographic column using the eluent of 2~3 times of column volumes, later, use institute
It states eluant, eluent to dissolve the vitamin E product after the decoloration of gained in step (a), in loading to above-mentioned chromatographic column.The chromatography
The diameter height ratio of column is 1:10~1:Between 100, and the height of chromatographic column is not less than 40cm.The diameter height of preferred column
Than being 1:20~1:Between 50.If the diameter height ratio of chromatographic column is less than 1:10 or chromatographic column height be less than 40 centimetres, can shadow
Ring the chromatographic purifying effect of sample；If the diameter height ratio of chromatographic column is higher than 1:100, then the flows decrease chromatographed reduces pure
Change efficiency.
In step (b), the column chromatography medium include be selected from by sephadex SephadexLH-20,
At least one of group of SephadexG-100, Sephacryl and Ago-Gel Sepharose compositions, preferably glucan
Gel SephadexLH-20.Sample loading volume be no more than column volume 10%, preferably loading volume for column volume 1~
5%.If loading volume is more than the 10% of column volume, decreased effectiveness is isolated and purified.
In step (b), the eluant, eluent includes being selected from by chloroform, methanol, dichloromethane, isopropanol and absolute ethyl alcohol group
Into at least one of group, preferably include to be selected from by chloroform:Methanol=3:1~3:2nd, dichloromethane:Methanol=3:1~3:2、
Dichloromethane:Isopropanol=3:1~3:2nd, chloroform:Isopropanol=3:1~3:2 and any one of the group of absolute ethyl alcohol composition,
By volume.Effectively vitamin E component with impurity can be detached using eluant, eluent of the present invention, and use other eluant, eluents
(such as n-hexane) is for gel chromatography vitamin E, then very weak without apparent purification effect or effect.
It in step (b), further includes and is detected using thin-layer chromatography, solvent is n-hexane:Ether:Acetic acid=8:2:
0.2, by volume.
The present invention vitamin E decoloration purification process the step of (c) in, be preferably concentrated under reduced pressure at no more than 50 DEG C
Eluent flow point to the organic solvent of gained eliminates in step (b), the vitamin E for obtaining decolourizing after purification.
In the decoloration purification process of the vitamin E of the present invention, still further comprise：It (d) will be after use in step (a)
Composite decoloring agent is recycled using organic solvent elution activation, and the organic solvent includes being selected from by absolute ethyl alcohol, more than 90%
Hydrous ethanol, n-hexane, normal heptane, petroleum ether, anhydrous ether, 1~5% acetic acid-ethanol solution (acetic acid by solution 1~
5% volume ratio is added in ethyl alcohol) and 1~5%KOH- ethanol solutions (KOH that 1~5g is added in 100ml ethyl alcohol) composition
At least one of group.
In some embodiments of the present invention, the obtained color and luster value of vitamin E product of the present invention for 12 hereinafter, it is preferred that
For 11 hereinafter, more preferably less than 10.
In some embodiments of the present invention, obtained the 25 of vitamin E product DEG C of the viscosity of the present invention is
1.42Pas hereinafter, and 70 DEG C of viscosity is 0.0503Pas hereinafter, it is preferred that 25 DEG C of viscosity is 0.130~1.42Pas,
And 70 DEG C of viscosity is 0.0156~0.0503Pas, more preferable 25 DEG C of viscosity is 0.130~1.26Pas, and 70 DEG C
Viscosity is 0.0156~0.0456Pas, and most preferably 25 DEG C of viscosity is 0.130~0.855Pas, and 70 DEG C of viscosity is
0.0156~0.0302Pas.
In some embodiments of the present invention, the obtained color and luster value of vitamin E product of the present invention for 12 hereinafter, it is preferred that
For 11 hereinafter, more preferably 10 hereinafter, and 25 DEG C of viscosity is 1.42Pas hereinafter, and 70 DEG C of viscosity is 0.0503Pas
Hereinafter, it is preferred that 25 DEG C of viscosity is 0.130~1.42Pas, and 70 DEG C of viscosity is 0.0156~0.0503Pas, it is more excellent
25 DEG C of viscosity is selected as 0.130~1.26Pas, and 70 DEG C of viscosity is 0.0156~0.0456Pas, most preferably 25 DEG C
Viscosity is 0.130~0.855Pas, and 70 DEG C of viscosity is 0.0156~0.0302Pas.
The embodiment of the present invention is given below.It should be noted that these embodiments are merely illustrative, the present invention is unlimited
In these embodiments.
In following embodiments of the present invention, the computational methods of the rate of recovery of vitamin E are as follows：
The rate of recovery=decoloration of vitamin E sample quality × decoloration sample content of vitamin E/(decoloration after purification after purification
Sample content of vitamin E before preceding sample quality × decoloration)
Wherein, sample quality refers to through composite decoloring agent decoloration and the sample quality of column chromatography after purification after purification for decoloration；
Purity in specific embodiment refers to the content of vitamin E.
Gardner (color and luster) value detection method is as follows：
It is measured using 3000 type colorimeter of Lovibond.
Method for detecting viscosity is as follows：
It is measured using MCR101 rheometers (Austrian Anton Paar Co., Ltd produces).
In following embodiments of the present invention, tocopherol content detection method is as follows in vitamin E sample：
With reference to the method for AOCS Ce8-89 (Reapproved-2009), detected using high performance liquid chromatography raw in sample
Educate the content of phenol.
In following embodiments of the present invention, atlapulgite, activated carbon, diatom that the composite decoloring agent that uses passes through purchase
Soil and magnesium silicate are uniformly mixed by a certain percentage to be prepared.
Embodiment 1
Take vitamin E sample (containing tocopherol 84.20%, wherein containing alpha-tocopherol 7.33%, betatocopherol 0.97%, γ-
Tocopherol 53.76%, Delta-Tocopherol 22.14%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g, it is anhydrous to add in 90g
Ethyl alcohol dissolves, and adds 9g composite decoloring agent (atlapulgites:Activated carbon:Diatomite:Magnesium silicate=100:50:50:30, w/w),
78 DEG C of condensing reflux decoloration 3h, filtering are heated to after stirring.Ethyl alcohol is distilled off in filtrate decompression, the vitamin E after being decolourized
Product.
50g sephadex SephadexLH-20 are taken, add in chloroform:Methanol=3:2 (v/v) 300ml are fully swollen, and are taken
Gel 150ml after swelling is fitted into chromatographic column (2cm × 50cm), and with 2 times of column volume stripping equilibria chromatographic columns.It takes above-mentioned de-
Vitamin E product 0.3238g after color adds in chloroform:Methanol=3:Loading after 2 (v/v) 3ml dissolvings, chromatographic column is with chloroform:First
Alcohol=3:2 (v/v) are eluted, and eluent is continuously collected and carries out thin-layer chromatography detection, and solvent is n-hexane:Ether:Acetic acid=
8:2:0.2 (v/v), collects the eluent flow point containing tocopherol, and be concentrated under reduced pressure into organic solvent at 50 DEG C after merging removes completely
It goes, the vitamin E product for obtaining decolourizing after purification.Composite decoloring agent after use with anhydrous ethanol elution twice, each dosage
Each 100g, filtering are repeated after drying and are utilized.It is 15 that sample purity, which is 84.20%, Gardner (color and luster) value, before decoloration, sample
It is 3.15Pas in 25 DEG C of viscosity, 70 DEG C of viscosity is 0.0876Pas；By the sample of decoloration after purification through efficient liquid
Phase chromatography (HPLC) detects, and purity rises to 98.29%, wherein containing alpha-tocopherol 8.55%, betatocopherol 1.13%, γ-life
Phenol 62.76%, Delta-Tocopherol 25.85% are educated, Gardner (color and luster) value is reduced to 10, and color and luster significantly shoals, and sample is at 25 DEG C
Viscosity is 0.832Pas, and 70 DEG C of viscosity is 0.0423Pas, and viscosity all drops significantly before relatively decolourizing at different temperature
It is low.In the present embodiment, the rate of recovery of vitamin E is 98.83%.
Embodiment 2
Vitamin E sample (containing alpha-tocopherol 91.42%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g is taken, is added
Enter 95% ethyl alcohol 90g dissolvings, add 6g composite decoloring agent (atlapulgites:Activated carbon:Diatomite:Magnesium silicate=100:70:
50:30, w/w) 78 DEG C of condensing reflux decoloration 3h, filtering, are heated to after stirring.Ethyl alcohol is distilled off in filtrate decompression, is decolourized
Vitamin E product afterwards.
200g sephadex SephadexLH-20 are taken, add in chloroform:Methanol=3:1 (v/v) 1000mL is fully swollen,
The gel 700mL after swelling is taken to be fitted into chromatographic column (3cm × 100cm), and with 2 times of column volume stripping equilibria chromatographic columns.It takes
The vitamin E product 1.4889g after decoloration is stated, adds in chloroform:Methanol=3:Loading after 1 (v/v) 10ml dissolvings, chromatographic column is with chlorine
It is imitative:Methanol=3:1 (v/v) is eluted, and eluent is continuously collected and carries out thin-layer chromatography detection, and solvent is n-hexane:Ether:Second
Acid=8:2:0.2 (v/v) collects the eluent flow point containing tocopherol, and it is complete at 50 DEG C to be concentrated under reduced pressure into organic solvent after merging
It is complete to remove, the vitamin E product for obtaining decolourizing after purification.Composite decoloring agent after use with 95% ethanol elution twice, every time
Each 100g of dosage, filtering are repeated after drying and are utilized.It is 14 that sample purity, which is 91.42%, Gardner (color and luster) value, before decoloration,
Sample is 2.29Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0607Pas；Through decoloration after purification sample through HPLC
Detection, purity rise to 97.88%, Gardner (color and luster) value and are reduced to 10, and color and luster significantly shoals, viscosity of the sample at 25 DEG C
For 1.25Pas, 70 DEG C of viscosity is 0.0448Pas, and viscosity all substantially reduces before relatively decolourizing at different temperature.At this
In embodiment, the rate of recovery of vitamin E is 97.55%.
Embodiment 3
Take vitamin E sample (containing tocopherol 51.04%, wherein containing alpha-tocopherol 12.33%, betatocopherol 1.89%,
Gamma-Tocopherol 32.36%, Delta-Tocopherol 4.46%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g, add in 60g without
Water-ethanol dissolves, and adds 9g composite decoloring agent (atlapulgites:Activated carbon:Diatomite:Magnesium silicate=100:80:30:10, w/
W), 80 DEG C of condensing reflux decoloration 2h, filtering are heated to after stirring.Ethyl alcohol is distilled off in filtrate decompression, the dimension life after being decolourized
Plain E products.
100g sephadex SephadexLH-20 are taken, add in dichloromethane:Methanol=3:1 (v/v) 500ml is fully molten
It is swollen, the gel 300ml after swelling is taken to be fitted into chromatographic column (2.5cm × 70cm), and with 2 times of column volume stripping equilibria chromatographic columns.
The vitamin E product 0.6238g after above-mentioned decoloration is taken, adds in dichloromethane:Methanol=3:Loading after 1 (v/v) 5ml dissolvings, color
Column is composed with dichloromethane:Methanol=3:1 (v/v) is eluted, and eluent is continuously collected and carries out thin-layer chromatography detection, and solvent is just
Hexane:Ether:Acetic acid=8:2:0.2 (v/v) collects the eluent flow point containing tocopherol, is concentrated under reduced pressure at 50 DEG C after merging
It is removed completely to organic solvent, the vitamin E product for obtaining decolourizing after purification.Composite decoloring agent after use is washed with 90% ethyl alcohol
De- each each 100g of dosage is filtered twice, recycling after drying.Sample purity is 51.04%, Gardner before decoloration
(color and luster) value is 14, and sample is 1.590Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0619Pas；It is pure by decolourizing
Sample after change is detected through HPLC, and purity rises to 92.27%, wherein containing alpha-tocopherol 22.28%, betatocopherol 3.42%,
Gamma-Tocopherol 58.50%, Delta-Tocopherol 8.07%, Gardner (color and luster) value are reduced to 10, and color and luster significantly shoals, and sample is 25
DEG C viscosity for 0.130Pas, 70 DEG C of viscosity is 0.0156Pas, before viscosity is relatively decolourized at different temperature all significantly
It reduces.In the present embodiment, the rate of recovery of vitamin E is 96.90%.
Embodiment 4
Vitamin E sample (containing alpha-tocopherol 91.07%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g is taken, is added
Enter 60g n-hexane dissolutions, add 12g composite decoloring agent (atlapulgites:Activated carbon:Diatomite:Magnesium silicate=100:100:
70:20, w/w) 50 DEG C of condensing reflux decoloration 1h, filtering, are heated to after stirring.N-hexane is distilled off in filtrate decompression, is taken off
Vitamin E product after color.
50g sephadex SephadexLH-20 are taken, add in 300ml dichloromethane:Methanol=3:2 (v/v) are fully molten
It is swollen, the gel 150ml after swelling is taken to be fitted into chromatographic column (1.5cm × 100cm), and with 2 times of column volume stripping equilibria chromatographic columns.
The vitamin E product 0.4252g after above-mentioned decoloration is taken, adds in dichloromethane:Methanol=3:Loading after 2 (v/v) 8ml dissolvings, color
Column is composed with dichloromethane:Methanol=3:2 (v/v) are eluted, and eluent is continuously collected and carries out thin-layer chromatography detection, and solvent is just
Hexane:Ether:Acetic acid=8:2:0.2 (v/v) collects the eluent flow point containing tocopherol, is concentrated under reduced pressure at 50 DEG C after merging
It is removed completely to organic solvent, the vitamin E product for obtaining decolourizing after purification.Composite decoloring agent after use is eluted with n-hexane
Twice, each 100g of each dosage, filtering are repeatable after drying to utilize.Sample purity is 91.07%, Gardner before decoloration
(color and luster) value is 14~15, and sample is 2.36Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0641Pas；By decoloration
Sample after purification is detected through HPLC, and purity rises to 96.58%, Gardner (color and luster) value and is reduced to 10, and color and luster significantly becomes
Shallow, sample is 1.24Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0434Pas, and viscosity is relatively de- at different temperature
It is all substantially reduced before color.In the present embodiment, the rate of recovery of vitamin E is 95.96%.
Embodiment 5
Vitamin E sample (containing alpha-tocopherol 91.07%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g is taken, is added
Enter the dissolving of 150g absolute ethyl alcohols, add 6g composite decoloring agent (atlapulgites:Activated carbon:Diatomite:Magnesium silicate=100:90:
70:50, w/w) 70 DEG C of condensing reflux decoloration 5h, filtering, are heated to after stirring.Ethyl alcohol is distilled off in filtrate decompression, after obtaining decoloration
Vitamin E product.
100g sephadex SephadexLH-20 are taken, add in 500ml dichloromethane:Isopropanol=3:2 (v/v) are abundant
Swelling takes the gel 300ml after swelling to be fitted into chromatographic column (2cm × 100cm), and with 2 times of column volume stripping equilibria chromatographic columns.
The vitamin E product 0.6880g after above-mentioned decoloration is taken, adds in dichloromethane:Isopropanol=3:Loading after 2 (v/v) 17ml dissolvings,
Chromatographic column is with dichloromethane:Isopropanol=3:2 (v/v) are eluted, and eluent is continuously collected and carries out thin-layer chromatography detection, solvent
For n-hexane:Ether:Acetic acid=8:2:0.2 (v/v) collects the eluent flow point containing tocopherol, is depressurized at 50 DEG C after merging
It is concentrated into organic solvent to remove completely, the vitamin E product for obtaining decolourizing after purification.The anhydrous second of composite decoloring agent after use
Alcohol elutes twice, each each 100g of dosage, filtering, repeatable after drying to utilize.Sample purity is 91.07% before decoloration,
Gardner (color and luster) value is 14~15, and sample is 2.36Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0641Pas；
It is detected by the sample to decolourize after purification through HPLC, purity rises to 97.24%, Gardner (color and luster) value and is reduced to 10, color and luster
It significantly shoals, sample is 1.42Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0503Pas, is glued at different temperature
Degree all substantially reduces before relatively decolourizing.In the present embodiment, the rate of recovery of vitamin E is 96.88%.
Embodiment 6
Take vitamin E sample (containing tocopherol 84.20%, wherein containing alpha-tocopherol 7.33%, betatocopherol 0.97%, γ-
Tocopherol 53.76%, Delta-Tocopherol 22.14%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g, add in 120g positive heptan
Alkane dissolves, and adds 15g composite decoloring agent (atlapulgites:Activated carbon:Diatomite:Magnesium silicate=100:50:50:20, w/w),
60 DEG C of condensing reflux decoloration 3h, filtering are heated to after stirring.Normal heptane is distilled off in filtrate decompression, the vitamin after being decolourized
E products.
100g sephadex SephadexLH-20 are taken, add in 500ml dichloromethane:Isopropanol=3:1 (v/v) is abundant
Swelling takes the gel 200ml after swelling to be fitted into chromatographic column (2.5cm × 50cm), and with 2 times of column volume stripping equilibria chromatographies
Column.The vitamin E product 0.2582g after above-mentioned decoloration is taken, adds in dichloromethane:Isopropanol=3:On after 1 (v/v) 3ml dissolvings
Sample, chromatographic column is with dichloromethane:Isopropanol=3:1 (v/v) is eluted, and eluent is continuously collected and carries out thin-layer chromatography detection, is opened up
Agent is opened as n-hexane:Ether:Acetic acid=8:2:0.2 (v/v) collects the eluent flow point containing tocopherol, after merging at 50 DEG C
It is concentrated under reduced pressure into organic solvent to remove completely, the vitamin E product for obtaining decolourizing after purification.Composite decoloring agent after use is with just
Heptane elutes twice, each each 100g of dosage, filtering, repeatable after drying to utilize.Sample purity is 84.20% before decoloration,
Gardner (color and luster) value is 15, and sample is 3.15Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0876Pas；By
Decoloration sample after purification is detected through HPLC, and purity rises to 96.73%, wherein containing alpha-tocopherol, 8.42%, betatocopherol
1.11%th, Gamma-Tocopherol 61.76%, Delta-Tocopherol 25.44%, Gardner (color and luster) value are reduced to 10, and color and luster significantly shoals,
Sample is 1.26Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0463Pas, and viscosity is relatively decolourized at different temperature
It is preceding all to substantially reduce.In the present embodiment, the rate of recovery of vitamin E is 95.34%.
Embodiment 7
Take vitamin E sample (containing tocopherol 30.68%, wherein containing alpha-tocopherol 7.12%, betatocopherol 1.10%, γ-
Tocopherol 19.45%, Delta-Tocopherol 3.01%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g, add in 120g just oneself
Alkane dissolves, and adds 6g composite decoloring agent (atlapulgites:Activated carbon:Diatomite:Magnesium silicate=100:80:30:10, w/w) it, stirs
40 DEG C of condensing reflux decoloration 2h, filtering are heated to after mixing.N-hexane is distilled off in filtrate decompression, the vitamin E after being decolourized
Product.
200g sephadex SephadexLH-20 are taken, add in chloroform:Isopropanol=3:2 (v/v) 1000ml are fully molten
It is swollen, the gel 700ml after swelling is taken to be fitted into chromatographic column (4cm × 60cm), and with 2 times of column volume stripping equilibria chromatographic columns.It takes
Vitamin E product 1.5088g after above-mentioned decoloration adds in chloroform:Isopropanol=3:Loading after 2 (v/v) 50ml dissolvings, chromatographic column
With chloroform:Isopropanol=3:2 (v/v) are eluted, and eluent is continuously collected and carries out thin-layer chromatography detection, and solvent is n-hexane:
Ether:Acetic acid=8:2:0.2 (v/v) collects the eluent flow point containing tocopherol, is concentrated under reduced pressure at 50 DEG C after merging organic
Solvent removes completely, the vitamin E product for obtaining decolourizing after purification.Composite decoloring agent after use is eluted twice with n-hexane,
Each 100g of each dosage, filtering are repeatable after drying to utilize.Sample purity is 30.68%, Gardner (color and luster) before decoloration
It is 15 to be worth, and sample is 1.23Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0574Pas；By the sample to decolourize after purification
Product are detected through HPLC, and purity rises to 78.60%, wherein containing alpha-tocopherol 18.24%, betatocopherol 2.83%, Gamma-Tocopherol
49.83%th, Delta-Tocopherol 7.70%, Gardner (color and luster) value are reduced to 10~11, and color and luster significantly shoals, and sample is at 25 DEG C
Viscosity is 0.26Pas, and 70 DEG C of viscosity is 0.0208Pas, and viscosity all substantially reduces before relatively decolourizing at different temperature.
In the present embodiment, the rate of recovery of vitamin E is 96.15%.
Embodiment 8
Take vitamin E sample (containing tocopherol 51.04%, wherein containing alpha-tocopherol 12.33%, betatocopherol 1.89%,
Gamma-Tocopherol 32.36%, Delta-Tocopherol 4.46%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g, add in 150g stones
Oily ether dissolving, adds 15g composite decoloring agent (atlapulgites:Activated carbon:Diatomite:Magnesium silicate=100:70:40:50, w/
W), 50 DEG C of condensing reflux decoloration 4h, filtering are heated to after stirring.Petroleum ether is distilled off in filtrate decompression, the dimension after being decolourized
Raw element E products.
100g sephadex SephadexLH-20 are taken, add in chloroform:Isopropanol=3:1 (v/v) 500ml is fully swollen,
The gel 300ml after swelling is taken to be fitted into chromatographic column (2.5cm × 75cm), and with 2 times of column volume stripping equilibria chromatographic columns.It takes
The vitamin E product 0.7281g after decoloration is stated, adds in chloroform:Isopropanol=3:1 (v/v) 8ml dissolving after loading, chromatographic column with
Chloroform:Isopropanol=3:1 (v/v) is eluted, and eluent is continuously collected and carries out thin-layer chromatography detection, and solvent is n-hexane:Second
Ether:Acetic acid=8:2:0.2 (v/v) collects the eluent flow point containing tocopherol, is concentrated under reduced pressure at 50 DEG C after merging organic molten
Agent removes completely, the vitamin E product for obtaining decolourizing after purification.Composite decoloring agent after use is eluted twice, often with petroleum ether
Secondary each 100g of dosage, filtering are repeatable after drying to utilize.Sample purity is 51.04%, Gardner (color and luster) value before decoloration
It is 14, sample is 1.590Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0619Pas；By the sample to decolourize after purification
Product are detected through HPLC, and purity rises to 94.38%, wherein containing alpha-tocopherol 22.79%, betatocopherol 3.50%, Gamma-Tocopherol
59.84%th, Delta-Tocopherol 8.25%, Gardner (color and luster) value are reduced to 10, and color and luster significantly shoals, viscosity of the sample at 25 DEG C
For 0.29Pas, 70 DEG C of viscosity is 0.0278Pas, and viscosity all substantially reduces before relatively decolourizing at different temperature.This reality
It applies in example, the rate of recovery of vitamin E is 95.43%.
Embodiment 9
Vitamin E sample (containing alpha-tocopherol 91.42%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g is taken, is added
Enter the dissolving of 90g anhydrous ethers, add 9g composite decoloring agent (atlapulgites:Activated carbon:Diatomite:Magnesium silicate=100:60:
60:40, w/w) 30 DEG C of decoloration 4h, filtering, are heated to after stirring.Ether is distilled off in filtrate decompression, the dimension life after being decolourized
Plain E products.
200g sephadex SephadexLH-20 are taken, absolute ethyl alcohol 1000ml is added in and is fully swollen, are taken solidifying after swelling
Glue 700ml is fitted into chromatographic column (3cm × 100cm), and with 2 times of column volume stripping equilibria chromatographic columns.Take the dimension after above-mentioned decoloration
Raw element E product 1.3361g, add in loading after absolute ethyl alcohol 10ml dissolvings, and chromatographic column is continuously received with anhydrous ethanol elution, eluent
Collect and carry out thin-layer chromatography detection, solvent is n-hexane:Ether:Acetic acid=8:2:0.2 (v/v), is collected containing tocopherol
Eluent flow point is concentrated under reduced pressure into absolute ethyl alcohol at 50 DEG C after merging and removes completely, the vitamin E production for obtaining decolourizing after purification
Product.Composite decoloring agent after use is eluted twice with anhydrous ether, each each 100g of dosage, filtering, repeatable profit after drying
With.It is 14 that sample purity, which is 91.42%, Gardner (color and luster) value, before decoloration, sample in 25 DEG C of viscosity for 2.29Pas, 70
DEG C viscosity be 0.0607Pas；It being detected by the sample to decolourize after purification through HPLC, purity rises to 95.77%,
Gardner (color and luster) value is reduced to 10~11, and color and luster significantly shoals, sample in 25 DEG C of viscosity for 1.26Pas, 70 DEG C viscous
It spends for 0.0447Pas, viscosity all substantially reduces before relatively decolourizing at different temperature.In the present embodiment, time of vitamin E
Yield is 95.72%.
Embodiment 10
Take vitamin E sample (containing tocopherol 84.20%, wherein containing alpha-tocopherol 7.33%, betatocopherol 0.97%, γ-
Tocopherol 53.76%, Delta-Tocopherol 22.14%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g, it is anhydrous to add in 30g
Ethyl alcohol dissolves, and adds 3g composite decoloring agent (atlapulgites:Activated carbon:Diatomite:Magnesium silicate=100:60:50:40, w/w),
78 DEG C of condensing reflux decoloration 3h, filtering are heated to after stirring.Ethyl alcohol is distilled off in filtrate decompression, the vitamin E after being decolourized
Product.
500g sephadex SephadexG-100 are taken, absolute ethyl alcohol 2000ml is added in and is fully swollen, are taken solidifying after swelling
Glue 1200ml is fitted into chromatographic column (6cm × 60cm), and with 2 times of column volume stripping equilibria chromatographic columns.Take the dimension after above-mentioned decoloration
Raw element E product 1.2882g, add in loading after absolute ethyl alcohol 7ml dissolvings, and chromatographic column is continuously received with anhydrous ethanol elution, eluent
Collect and carry out thin-layer chromatography detection, solvent is n-hexane:Ether:Acetic acid=8:2:0.2 (v/v), is collected containing tocopherol
Eluent flow point is concentrated under reduced pressure into organic solvent at 50 DEG C after merging and removes completely, the vitamin E production for obtaining decolourizing after purification
Product.With anhydrous ethanol elution twice, each each 100g of dosage, filtering repeats profit to composite decoloring agent after use after drying
With.It is 15 that sample purity, which is 84.20%, Gardner (color and luster) value, before decoloration, sample in 25 DEG C of viscosity for 3.15Pas, 70
DEG C viscosity be 0.0876Pas；It is detected by the sample to decolourize after purification through HPLC, purity rises to 97.24%, wherein containing
Alpha-tocopherol 8.46%, betatocopherol 1.12%, Gamma-Tocopherol 62.09%, Delta-Tocopherol 25.57%, Gardner (color and luster)
Value is reduced to 10~11, and color and luster significantly shoals, and sample is 1.25Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is
0.0435Pas is substantially reduced before viscosity relatively decoloration at different temperature.In the present embodiment, the rate of recovery of vitamin E
It is 95.29%.
Embodiment 11
Take vitamin E sample (containing tocopherol 30.68%, wherein containing alpha-tocopherol 7.12%, betatocopherol 1.10%, γ-
Tocopherol 19.45%, Delta-Tocopherol 3.01%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g, add in the anhydrous second of 60g
Ether dissolves, and adds 9g composite decoloring agent (atlapulgites:Activated carbon:Diatomite:Magnesium silicate=100:70:40:40, w/w) it, stirs
30 DEG C of decoloration 5h, filtering are heated to after mixing.Ether is distilled off in filtrate decompression, the vitamin E product after being decolourized.
50g sephadex SephadexG-100 and 50g Sephacryl is taken to mix, it is abundant to add in absolute ethyl alcohol 500ml
Swelling takes the gel 200ml after swelling to be fitted into chromatographic column (1.5cm × 120cm), and with 2 times of column volume stripping equilibria chromatographies
Column.The vitamin E product 0.6970g after above-mentioned decoloration is taken, adds in loading after absolute ethyl alcohol 8ml dissolvings, chromatographic column is with anhydrous second
Alcohol elutes, and eluent is continuously collected and carries out thin-layer chromatography detection, and solvent is n-hexane:Ether:Acetic acid=8:2:0.2(v/
V), the eluent flow point containing tocopherol is collected, be concentrated under reduced pressure into organic solvent at 50 DEG C after merging removes completely, is decolourized
Vitamin E product after purification.With 5% acetic acid-ethanol solution elution twice, each dosage is each for composite decoloring agent after use
100g, then with anhydrous ethanol elution to neutrality, filtering is repeatable after drying to utilize.Sample purity is 30.68% before decoloration,
Gardner (color and luster) value is 15, and sample is 1.23Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0574Pas；By
The sample of decoloration after purification is detected through HPLC, and purity rises to 72.72%, wherein containing alpha-tocopherol 16.87%, betatocopherol
2.62%th, Gamma-Tocopherol 46.10%, Delta-Tocopherol 7.13%Gardner (color and luster) value are reduced to 10~11, and color and luster significantly becomes
Shallow, sample is 0.22Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0182Pas, and viscosity is relatively de- at different temperature
It is all substantially reduced before color.In the present embodiment, the rate of recovery of vitamin E is 95.63%.
Embodiment 12
Take vitamin E sample (containing tocopherol 51.04%, wherein containing alpha-tocopherol 12.33%, betatocopherol 1.89%,
Gamma-Tocopherol 32.36%, Delta-Tocopherol 4.46%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g, it adds in
120g90% ethyl alcohol dissolves, and adds 12g composite decoloring agent (atlapulgites:Activated carbon:Diatomite:Magnesium silicate=100:70:
50:30, w/w) 80 DEG C of condensing reflux decoloration 2h, filtering, are heated to after stirring.Ethyl alcohol is distilled off in filtrate decompression, is decolourized
Vitamin E product afterwards.
300g Ago-Gel Sepharose are taken, absolute ethyl alcohol 2000ml is added in and is fully swollen, take the gel after swelling
700ml is fitted into chromatographic column (3cm × 120cm), and with 2 times of column volume stripping equilibria chromatographic columns.The dimension after above-mentioned decoloration is taken to give birth to
Plain E products 1.6832g, adds in loading after the dissolving of 30ml absolute ethyl alcohols, and chromatographic column is continuously collected with anhydrous ethanol elution, eluent
And thin-layer chromatography detection is carried out, solvent is n-hexane:Ether:Acetic acid=8:2:0.2 (v/v), collects washing containing tocopherol
De- liquid stream point, is concentrated under reduced pressure into organic solvent at 50 DEG C after merging and removes completely, the vitamin E product for obtaining decolourizing after purification.
Composite decoloring agent after use is eluted twice with 5%KOH ethanol solutions, each each 100g of dosage, then with anhydrous ethanol elution extremely
Neutrality, filtering are repeatable after drying to utilize.It is 14 that sample purity, which is 51.04%, Gardner (color and luster) value, before decoloration, sample
It is 1.59Pas in 25 DEG C of viscosity, 70 DEG C of viscosity is 0.0619Pas；It is examined by the sample to decolourize after purification through HPLC
It surveys, purity rises to 94.87%, wherein containing α-fertility 22.91%, betatocopherol 3.52%, Gamma-Tocopherol 60.15%, δ-life
Phenol 8.29% is educated, Gardner (color and luster) value is reduced to 10~11, and color and luster significantly shoals, and sample is in 25 DEG C of viscosity
0.33Pas, 70 DEG C of viscosity is 0.0302Pas, and viscosity all substantially reduces before relatively decolourizing at different temperature.In this reality
It applies in example, the rate of recovery of vitamin E is 95.28%.
Embodiment 13
Take vitamin E sample (containing tocopherol 84.20%, wherein containing alpha-tocopherol 7.33%, betatocopherol 0.97%, γ-
Tocopherol 53.76%, Delta-Tocopherol 22.14%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g, it is anhydrous to add in 90g
Ethyl alcohol dissolves, and adds 9g composite decoloring agent (atlapulgites:Activated carbon:Diatomite:Magnesium silicate=100:70:50:25, w/w),
78 DEG C of condensing reflux decoloration 3h, filtering are heated to after stirring.Ethyl alcohol is distilled off in filtrate decompression, the vitamin E after being decolourized
Product.
50g sephadex SephadexLH-20 are taken, add in chloroform:Methanol=3:2 (v/v) 300ml are fully swollen, and are taken
Gel 150ml after swelling is fitted into chromatographic column (2cm × 50cm), and with 2 times of column volume stripping equilibria chromatographic columns.It takes above-mentioned de-
Vitamin E product 0.4018g after color adds in chloroform:Methanol=3:Loading after 2 (v/v) 3ml dissolvings, chromatographic column is with chloroform:First
Alcohol=3:2 (v/v) are eluted, and eluent is continuously collected and carries out thin-layer chromatography detection, and solvent is n-hexane:Ether:Acetic acid=
8:2:0.2 (v/v), collects the eluent flow point containing tocopherol, and be concentrated under reduced pressure into organic solvent at 50 DEG C after merging removes completely
It goes, the vitamin E product for obtaining decolourizing after purification.Composite decoloring agent after use with anhydrous ethanol elution twice, each dosage
Each 100g, filtering are repeated after drying and are utilized.It is 15 that sample purity, which is 84.20%, Gardner (color and luster) value, before decoloration, sample
It is 3.15Pas in 25 DEG C of viscosity, 70 DEG C of viscosity is 0.0876Pas；It is examined by the sample to decolourize after purification through HPLC
It surveys, purity rises to 97.39%, Gardner (color and luster) value and is reduced to 10, and color and luster significantly shoals, and sample is in 25 DEG C of viscosity
0.855Pas, 70 DEG C of viscosity is 0.0429Pas, and viscosity all substantially reduces before relatively decolourizing at different temperature.At this
In embodiment, the rate of recovery of vitamin E is 98.23%.
Embodiment 14
Vitamin E sample (containing alpha-tocopherol 91.42%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g is taken, is added
Enter 95% ethyl alcohol 90g dissolvings, add 6g composite decoloring agent (atlapulgites:Activated carbon:Diatomite:Magnesium silicate=100:60:
50:35, w/w) 78 DEG C of condensing reflux decoloration 3h, filtering, are heated to after stirring.Ethyl alcohol is distilled off in filtrate decompression, is decolourized
Vitamin E product afterwards.
200g sephadex SephadexLH-20 are taken, add in chloroform:Methanol=3:1 (v/v) 1000mL is fully swollen,
The gel 700mL after swelling is taken to be fitted into chromatographic column (3cm × 100cm), and with 2 times of column volume stripping equilibria chromatographic columns.It takes
The vitamin E product 1.3297g after decoloration is stated, adds in chloroform:Methanol=3:Loading after 1 (v/v) 10ml dissolvings, chromatographic column is with chlorine
It is imitative:Methanol=3:1 (v/v) is eluted, and eluent is continuously collected and carries out thin-layer chromatography detection, and solvent is n-hexane:Ether:Second
Acid=8:2:0.2 (v/v) collects the eluent flow point containing tocopherol, and it is complete at 50 DEG C to be concentrated under reduced pressure into organic solvent after merging
It is complete to remove, the vitamin E product for obtaining decolourizing after purification.Composite decoloring agent after use with 95% ethanol elution twice, every time
Each 100g of dosage, filtering are repeated after drying and are utilized.It is 14 that sample purity, which is 91.42%, Gardner (color and luster) value, before decoloration,
Sample is 2.29Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0607Pas；Through decoloration after purification sample through HPLC
Detection, purity rise to 97.54%, Gardner (color and luster) value and are reduced to 10~11, and color and luster significantly shoals, and sample is at 25 DEG C
Viscosity is 1.26Pas, and 70 DEG C of viscosity is 0.0456Pas, and viscosity all substantially reduces before relatively decolourizing at different temperature.
In the present embodiment, the rate of recovery of vitamin E is 97.26%.
Comparative example 1
Take vitamin E sample (containing tocopherol 84.20%, wherein containing alpha-tocopherol 7.33%, betatocopherol 0.97%, γ-
Tocopherol 53.76%, Delta-Tocopherol 22.14%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g, it is anhydrous to add in 90g
Ethyl alcohol dissolves, and adds 9g composite decoloring agent (atlapulgites:Activated carbon:Diatomite:Magnesium silicate=100:50:50:30, w/w),
Stirring is heated to 78 DEG C of condensing reflux decoloration 3h, filtering.Ethyl alcohol is distilled off in filtrate decompression, the vitamin E production after being decolourized
Product.
100g sephadex SephadexLH-20 are taken, 500ml n-hexanes is added in and is fully swollen, take the gel after swelling
200ml is fitted into chromatographic column (2.5cm × 50cm), and with 2 times of column volume stripping equilibria chromatographic columns.The dimension after above-mentioned decoloration is taken to give birth to
Plain E products 0.3068g adds in loading after n-hexane 5ml dissolvings, and chromatographic column is eluted with n-hexane, and eluent is continuously collected and gone forward side by side
Row thin-layer chromatography detects, and solvent is n-hexane:Ether:Acetic acid=8:2:0.2 (v/v), collects the eluent containing tocopherol
Flow point is concentrated under reduced pressure into organic solvent at 50 DEG C after merging and removes completely, the vitamin E product for obtaining decolourizing after purification.Decoloration
Preceding sample purity is that 84.20%, Gardner (color and luster) value is 15, sample in 25 DEG C of viscosity for 3.15Pas, 70 DEG C viscous
It spends for 0.0876Pas；It is detected by the sample to decolourize after purification through HPLC, purity 85.92%, wherein containing alpha-tocopherol
7.48%th, betatocopherol 0.99%, Gamma-Tocopherol 54.86%, Delta-Tocopherol 22.59%, Gardner (color and luster) value are 12, sample
Product are 2.08Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0576Pas, and the rate of recovery of vitamin E is 97.22%.
Comparative example 2
300g Ago-Gel Sepharose are taken, absolute ethyl alcohol 2000ml is added in and is fully swollen, take the gel after swelling
700ml is fitted into chromatographic column (3cm × 120cm), and with 2 times of column volume stripping equilibria chromatographic columns.Vitamin E sample is taken (containing life
Phenol 51.04% is educated, wherein containing alpha-tocopherol 12.33%, betatocopherol 1.89%, Gamma-Tocopherol 32.36%, Delta-Tocopherol
4.46%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 1.5281g, add in loading after the dissolving of 10ml absolute ethyl alcohols, chromatography
Column is with anhydrous ethanol elution, and eluent is continuously collected and carries out thin-layer chromatography detection, and solvent is n-hexane:Ether:Acetic acid=
8:2:0.2 (v/v), collects the eluent flow point containing tocopherol, and be concentrated under reduced pressure into organic solvent at 50 DEG C after merging removes completely
It goes, the vitamin E product for obtaining decolourizing after purification.It is 14 that sample purity, which is 51.04%, Gardner (color and luster) value, before decoloration, sample
Product are 1.59Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0619Pas；By the sample of decoloration after purification through HPLC
Detection, purity 83.87%, wherein containing alpha-tocopherol 20.25%, betatocopherol 3.11%, Gamma-Tocopherol 53.55%, δ-life
Phenol 6.96% is educated, Gardner (color and luster) value is 12~13, and sample is 1.53Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is
0.0602Pas, the rate of recovery of vitamin E is 96.81%.
Comparative example 3
Take vitamin E sample (containing tocopherol 84.20%, wherein containing alpha-tocopherol 7.33%, betatocopherol 0.97%, γ-
Tocopherol 53.76%, Delta-Tocopherol 22.14%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g, add in 120g positive heptan
Alkane dissolves, and adds 15g activated carbons, and 60 DEG C of condensing reflux decoloration 3h, filtering are heated to after stirring.Filtrate decompression is distilled off just
Heptane, the vitamin E product after being decolourized.
100g sephadex SephadexLH-20 are taken, add in 500ml dichloromethane:Isopropanol=3:1 (v/v) is abundant
Swelling takes the gel 200ml after swelling to be fitted into chromatographic column (2.5cm × 50cm), and with 2 times of column volume stripping equilibria chromatographies
Column.The vitamin E product 0.5018g after above-mentioned decoloration is taken, adds in dichloromethane:Isopropanol=3:On after 1 (v/v) 5ml dissolvings
Sample, chromatographic column is with dichloromethane:Isopropanol=3:1 (v/v) is eluted, and eluent is continuously collected and carries out thin-layer chromatography detection, is opened up
Agent is opened as n-hexane:Ether:Acetic acid=8:2:0.2 (v/v) collects the eluent flow point containing tocopherol, after merging at 50 DEG C
It is concentrated under reduced pressure into organic solvent to remove completely, the vitamin E product for obtaining decolourizing after purification.Sample purity is before decoloration
84.20%, Gardner (color and luster) value is 15, and sample is 3.15Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is
0.0876Pa·s；It is detected by the sample to decolourize after purification through HPLC, purity 92.98%, wherein containing alpha-tocopherol
8.09%th, betatocopherol 1.07%, Gamma-Tocopherol 59.37%, Delta-Tocopherol 24.45%, Gardner (color and luster) value are 13, sample
Product are 3.14Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0871Pas, and the rate of recovery of vitamin E is 96.83%.
Comparative example 4
Vitamin E sample (containing alpha-tocopherol 91.07%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g is taken, is added
Enter 60g n-hexane dissolutions, add 12g composite decoloring agent (atlapulgites:Activated carbon=2:1, w/w) 50, are heated to after stirring
DEG C, condensing reflux decoloration 1h, filtering.N-hexane is distilled off in filtrate decompression, the vitamin E product after being decolourized.
100g sephadex SephadexLH-20 are taken, add in dichloromethane:Methanol=3:2 (v/v) 500ml are fully molten
It is swollen, the gel 300ml after swelling is taken to be fitted into chromatographic column (2.5cm × 75cm), and with 2 times of column volume stripping equilibria chromatographic columns.
The vitamin E product 0.8031g after above-mentioned decoloration is taken, adds in dichloromethane:Methanol=3:Loading after 2 (v/v) 8ml dissolvings, color
Column is composed with dichloromethane:Methanol=3:2 (v/v) are eluted, and eluent is continuously collected and carries out thin-layer chromatography detection, and solvent is just
Hexane:Ether:Acetic acid=8:2:0.2 (v/v) collects the eluent flow point containing tocopherol, is concentrated under reduced pressure at 50 DEG C after merging
It is removed completely to organic solvent, the vitamin E product for obtaining decolourizing after purification.Sample purity is 91.07% before decoloration,
Gardner (color and luster) value is 14~15, and sample is 2.36Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0641Pas；
It is detected by the sample to decolourize after purification through HPLC, purity 93.57%, Gardner (color and luster) value is 13, and sample is at 25 DEG C
Viscosity is 2.26Pas, and 70 DEG C of viscosity is 0.0604Pas, and the rate of recovery of vitamin E is 92.72%.
Comparative example 5
Vitamin E sample (containing alpha-tocopherol 91.07%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g is taken, is added
Enter the dissolving of 150g absolute ethyl alcohols, add 6g composite decoloring agent (atlapulgites:Activated carbon:Diatomite:Magnesium silicate=100:40:
80:60, w/w) 70 DEG C of decoloration 5h, filtering, are heated to after stirring.Ethyl alcohol is distilled off in filtrate decompression, the dimension life after being decolourized
Plain E products.
300g sephadex SephadexLH-20 are taken, add in dichloromethane:Isopropanol=3:2 (v/v) 2000ml are abundant
Swelling takes the gel 700ml after swelling to be fitted into chromatographic column (3cm × 120cm), and with 2 times of column volume stripping equilibria chromatographic columns.
The vitamin E product 2.0137g after above-mentioned decoloration is taken, adds in dichloromethane:Isopropanol=3:Loading after 2 (v/v) 10ml dissolvings,
Chromatographic column is with dichloromethane:Isopropanol=3:2 (v/v) are eluted, and eluent is continuously collected and carries out thin-layer chromatography detection, solvent
For n-hexane:Ether:Acetic acid=8:2:0.2 (v/v) collects the eluent flow point containing tocopherol, is depressurized at 50 DEG C after merging
It is concentrated into organic solvent to remove completely, the vitamin E product for obtaining decolourizing after purification.Sample purity is 91.07% before decoloration,
Gardner (color and luster) value is 14~15, and sample is 2.36Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0641Pas；
It is detected by the sample to decolourize after purification through HPLC, purity 94.55%, Gardner (color and luster) value is 13, and sample is at 25 DEG C
Viscosity is 2.14Pas, and 70 DEG C of viscosity is 0.0598Pas, and the rate of recovery of vitamin E is 93.11%.
Comparative example 6
Take vitamin E sample (containing tocopherol 51.04%, wherein containing alpha-tocopherol 12.33%, betatocopherol 1.89%,
Gamma-Tocopherol 32.36%, Delta-Tocopherol 4.46%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g, add in just oneself
Alkane:Absolute ethyl alcohol=8:1 (v/v) 50ml dissolves, and silicagel column (silica filler 500g) is crossed, with n-hexane:Absolute ethyl alcohol=8:1
(v/v) it elutes, eluent is continuously collected and carries out thin-layer chromatography detection, and solvent is n-hexane:Ether:Acetic acid=8:2:0.2
(v/v), the eluent flow point containing tocopherol is collected, 12g composite decoloring agent (atlapulgites are added in after merging:Activated carbon:Diatom
Soil:Magnesium silicate=100:70:50:30, w/w) it decolourizes, 80 DEG C of condensing reflux decoloration 2h is heated to after stirring, destainer subtracts
Pressure is concentrated into organic solvent and removes completely, the vitamin E product for obtaining decolourizing after purification.Sample purity is 51.04% before decoloration,
Gardner (color and luster) value is 14, and sample is 1.59Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0619Pas；By
The sample of decoloration after purification is detected through HPLC, purity 97.14%, wherein containing alpha-tocopherol 23.46%, betatocopherol
3.60%th, Gamma-Tocopherol 61.59%, Delta-Tocopherol 8.49%, Gardner (color and luster) value are 10~11, and sample is viscous at 25 DEG C
It spends for 0.29Pas, 70 DEG C of viscosity is 0.0315Pas, and the rate of recovery of vitamin E is 73.55%.
Comparative example 7
Take vitamin E sample (containing tocopherol 30.68%, wherein containing alpha-tocopherol 7.12%, betatocopherol 1.10%, γ-
Tocopherol 19.45%, Delta-Tocopherol 3.01%, purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g, add in 120g just oneself
Alkane dissolves, and adds 6g composite decoloring agent (atlapulgites:Activated carbon:Diatomite:Magnesium silicate=100:80:30:10, w/w) it, stirs
40 DEG C of condensing reflux decoloration 2h, filtering are heated to after mixing.N-hexane is distilled off in filtrate decompression, the vitamin E after being decolourized
Product.
200g macroreticular resin D101 are taken, to be fitted into chromatographic column after 500ml soaked in absolute ethyl alcohol, and are washed with 2 times of column volumes
De- balance chromatographic column.The vitamin E product 10g after decoloration is taken, adds in loading after absolute ethyl alcohol 30ml dissolvings, chromatographic column is with anhydrous
Ethanol elution, eluent are continuously collected and carry out thin-layer chromatography detection, and solvent is n-hexane:Ether:Acetic acid=8:2:0.2
(v/v), the eluent flow point containing tocopherol is collected, be concentrated under reduced pressure into organic solvent at 50 DEG C after merging removes completely, obtains
The vitamin E product of decoloration after purification.It is 15 that sample purity, which is 30.68%, Gardner (color and luster) value, before decoloration, and sample is 25
DEG C viscosity for 1.23Pas, 70 DEG C of viscosity is 0.0574Pas；It is detected by the sample to decolourize after purification through HPLC, it is pure
It is 36.75% to spend, wherein containing alpha-tocopherol 8.53%, betatocopherol 1.32%, Gamma-Tocopherol 23.30%, Delta-Tocopherol
3.60%, Gardner (color and luster) value is 13, and sample is 0.86Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0334Pa
S, the rate of recovery of vitamin E is 88.20%.
Comparative example 8
500g sephadex SephadexLH-20 are taken, with 3000ml chloroforms:Isopropanol=3:After 2 (v/v) fully swellings
It is fitted into chromatographic column (7cm × 100cm), and with 2 times of column volume stripping equilibria chromatographic columns.Vitamin E sample is taken (containing tocopherol
30.68%, wherein containing alpha-tocopherol 7.12%, betatocopherol 1.10%, Gamma-Tocopherol 19.45%, Delta-Tocopherol 3.01%,
Purchased from Jiangsu Chunzhigu Biological Products Co., Ltd.) 30g, add in chloroform:Isopropanol=3:Loading after 2 (v/v) 60ml dissolvings, color
Column is composed with chloroform:Isopropanol=3:2 (v/v) are eluted, and eluent continuously collects and carry out thin-layer chromatography detection, solvent for just oneself
Alkane:Ether:Acetic acid=8:2:0.2 (v/v) collects the eluent flow point containing tocopherol, is concentrated under reduced pressure at 50 DEG C after merging
Organic solvent removes completely.Hereafter sample adds in 120g n-hexane dissolutions, adds 6g composite decoloring agent (atlapulgites:Activity
Charcoal:Diatomite:Magnesium silicate=100:80:30:10, w/w) 40 DEG C of condensing reflux decoloration 2h, filtering, are heated to after stirring.Filtrate
Vacuum distillation removes n-hexane, the vitamin E product for obtaining decolourizing after purification.Sample purity is 30.68% before decoloration,
Gardner (color and luster) value is 15, and sample is 1.23Pas in 25 DEG C of viscosity, and 70 DEG C of viscosity is 0.0574Pas；By
The sample of decoloration after purification is detected through HPLC, purity 67.33%, wherein containing alpha-tocopherol 15.62%, betatocopherol
2.42%th, Gamma-Tocopherol 42.69%, Delta-Tocopherol 6.6%, Gardner (color and luster) value are reduced to 12, and sample is viscous at 25 DEG C
It spends for 0.31Pas, 70 DEG C of viscosity is 0.0284Pas, and the rate of recovery of vitamin E is 90.51%.
By the embodiment of the present invention 1 and comparative example 1 as can be seen that when other conditions are constant, and use the present invention
Except other solvent systems carry out gel column elution when, the purity of sample is not significantly improved.
It is walked by the embodiment of the present invention 12 and comparative example 2 as can be seen that omitting adsorption bleaching before column chromatography
When rapid, Gardner (color and luster) values and viscosity of sample do not reduce significantly, and purity is also below there is adsorption bleaching step
, therefore show that adsorption bleaching step is essential in this patent.
By the comparative example 3,4,5 of the present invention as can be seen that when decolorising agent used is single adsorption agent (such as activity
Charcoal) or decolorising agent composition be not the present invention composite decoloring agent (such as atlapulgite：Activated carbon=2:1) or decolorising agent composition with
The present invention is identical, but when decolorising agent ratio does not fall within the scope of the present invention, and Gardner (color and luster) values and viscosity of sample do not have
Apparent to reduce, decoloration purification effect is below composite decoloring agent of the present invention.
By the embodiment of the present invention 12 and comparative example 6 as can be seen that when being used as chromatography media using silica gel, sample
The purification effect of product and the present invention are substantially suitable, but silica gel has sample stronger suction-operated, therefore the rate of recovery of sample
Chromatography media gel substantially less than of the present invention.
By the embodiment of the present invention 7 and comparative example 7 as can be seen that when being used as chromatography media using macroreticular resin
When, the purity of sample is not obviously improved.
By the embodiment of the present invention 7 and comparative example 8 as can be seen that layer after the first adsorption bleaching used in the present invention
The method of analysis purifying can significantly improve the purity of sample, significantly reduce Gardner (color and luster) values and viscosity of sample, if first
Rear decoloring is chromatographed, then the effect for purifying of decolourizing will weaken, and the rate of recovery of sample reduces.
It can be seen that by the experimental result of above example and comparative example pure for the decoloration of vitamin E product
Change, only using composite decoloring agent described in the present invention, chromatography media, eluting solvent and other parameter, can be only achieved
Ideal decoloration purification effect, and use other experiment parameters except the present invention, then the present invention can not be realized to vitamin E
Decolourize purification effect.
Claims (14)
1. a kind of decoloration purification process of vitamin E, the described method comprises the following steps：
(a) composite decoloring agent is provided, decolorization is carried out to vitamin E product；
(b) as column chromatography and with the vitamin E product after the decoloration obtained by eluent step (a), eluent is collected
Flow point；
(c) the eluent flow point of gained in step (b) is concentrated, the vitamin E for obtaining decolourizing after purification, wherein, in step (a)
In, the composite decoloring agent is atlapulgite:Activated carbon:Diatomite:Magnesium silicate=100:50~100:30~70:10~50,
By mass.
2. the decoloration purification process of vitamin E according to claim 1, which is characterized in that in step (a), the dimension
Raw element E products contain alpha-tocopherol, alpha-tocotrienol, betatocopherol, β-tocotrienols, Gamma-Tocopherol, γ-fertility three
Any one or a few in alkene phenol, Delta-Tocopherol, δ-tocotrienols, the content of total tocopherol is more than 30%.
3. the decoloration purification process of vitamin E according to claim 1 or 2, which is characterized in that described in step (a)
Composite decoloring agent is atlapulgite:Activated carbon:Diatomite:Magnesium silicate=100:50~70:40~60:25~35, by mass.
4. the decoloration purification process of vitamin E according to claim 1 or 2, which is characterized in that described in step (a)
The addition of composite decoloring agent is the 10~50% of the vitamin E product quality.
5. the decoloration purification process of vitamin E according to claim 4, which is characterized in that described multiple in step (a)
The addition for closing decolorising agent is the 20~40% of the vitamin E product quality.
6. the decoloration purification process of vitamin E according to claim 1 or 2, which is characterized in that in step (b), also wrap
It includes before with the vitamin E product after the decoloration of gained in the eluent step (a), is impregnated using the eluant, eluent
Column chromatography medium, stripping equilibria chromatographic column.
7. the decoloration purification process of vitamin E according to claim 1 or 2, which is characterized in that in step (b), also wrap
It includes before with the vitamin E product after the decoloration of gained in the eluent step (a), will be walked using the eluant, eluent
Suddenly the vitamin E product dissolving in (a) after the decoloration of gained.
8. the decoloration purification process of vitamin E according to claim 6, which is characterized in that the column chromatography medium includes
Selected from by sephadex SephadexLH-20, SephadexG-100, Sephacryl and Ago-Gel Sepharose groups
Into at least one of group.
9. the decoloration purification process of vitamin E according to claim 8, which is characterized in that the column chromatography medium is Portugal
Polysaccharide gel SephadexLH-20.
10. the decoloration purification process of vitamin E according to claim 1 or 2, which is characterized in that in step (b), institute
Eluant, eluent is stated to include being selected from least one of group being made of chloroform, methanol, dichloromethane, isopropanol and absolute ethyl alcohol.
11. the decoloration purification process of vitamin E according to claim 10, which is characterized in that described in step (b)
Eluant, eluent includes being selected from by chloroform:Methanol=3:1~3:2nd, dichloromethane:Methanol=3:1~3:2nd, dichloromethane:Isopropanol=
3:1~3:2nd, chloroform:Isopropanol=3:1~3:2 and any one of the group of absolute ethyl alcohol composition, by volume.
12. a kind of decolorising agent, which is characterized in that the decolorising agent is atlapulgite:Activated carbon:Diatomite:Magnesium silicate=100:
50~100:30~70:10~50, by mass.
13. decolorising agent according to claim 12, which is characterized in that the decolorising agent is atlapulgite:Activated carbon:Diatom
Soil:Magnesium silicate=100:50~70:40~60:25~35, by mass.
14. the purposes that decolorising agent purifies for vitamin E decoloration according to claim 12 or 13.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410640346.8A CN105585552B (en) | 2014-11-13 | 2014-11-13 | A kind of decoloration purification process of vitamin E |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410640346.8A CN105585552B (en) | 2014-11-13 | 2014-11-13 | A kind of decoloration purification process of vitamin E |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105585552A CN105585552A (en) | 2016-05-18 |
| CN105585552B true CN105585552B (en) | 2018-06-26 |
Family
ID=55925493
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410640346.8A Active CN105585552B (en) | 2014-11-13 | 2014-11-13 | A kind of decoloration purification process of vitamin E |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105585552B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109401838A (en) * | 2017-08-16 | 2019-03-01 | 上海茉笠品牌管理有限公司 | The discoloration method of jasmine essential oil |
| CN110327884B (en) * | 2019-07-13 | 2022-04-01 | 安徽科技学院 | Composite material for removing vitamin C solution pigment, preparation method and decoloring method thereof |
| CN114644609A (en) * | 2020-12-18 | 2022-06-21 | 丰益生物科技(江苏)有限公司 | Method for extracting natural vitamin E from byproduct residual oil |
| CN114831934B (en) * | 2022-05-11 | 2023-05-26 | 回音必集团抚州制药有限公司 | Preparation method of nicardipine hydrochloride injection |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1263096A (en) * | 1999-12-24 | 2000-08-16 | 上海交通大学 | Method for raising natural vitamin E concentrate transparency and fluidity |
| CN101921254A (en) * | 2010-08-12 | 2010-12-22 | 江苏省中国科学院植物研究所 | Method for extracting natural vitamin E from blackberry seeds |
| 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% |
| 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 |
| CN103965156A (en) * | 2014-04-16 | 2014-08-06 | 江苏玺鑫维生素有限公司 | Column chromatography for purification of natural vitamin E |
-
2014
- 2014-11-13 CN CN201410640346.8A patent/CN105585552B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1263096A (en) * | 1999-12-24 | 2000-08-16 | 上海交通大学 | Method for raising natural vitamin E concentrate transparency and fluidity |
| CN101921254A (en) * | 2010-08-12 | 2010-12-22 | 江苏省中国科学院植物研究所 | Method for extracting natural vitamin E from blackberry seeds |
| 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% |
| 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 |
| CN103965156A (en) * | 2014-04-16 | 2014-08-06 | 江苏玺鑫维生素有限公司 | Column chromatography for purification of natural vitamin E |
Non-Patent Citations (1)
| Title |
|---|
| 天然α-生育酚脱色工艺研究;陈隽义;《中国学位论文全文数据库》;20101018;第一至五章 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105585552A (en) | 2016-05-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Liu et al. | Preparative separation and purification of lycopene from tomato skins extracts by macroporous adsorption resins | |
| JP3547741B2 (en) | High cis-β-carotene composition | |
| CN105585552B (en) | A kind of decoloration purification process of vitamin E | |
| DE60103431T2 (en) | A method for the chromatographic isolation of isomers of vitamin E. | |
| CN102911138B (en) | The extracting and purifying method of fucoxanthin in a kind of brown alga | |
| CN111039761B (en) | Method for purifying cannabidiol | |
| EP1310478A1 (en) | Process for producing oleanolic acid and/or maslinic acid | |
| JP2009120494A (en) | Method for producing brown algae extract highly containing fucoxanthin | |
| CN104435134B (en) | A kind of method that flavonoids is extracted in the seed peel from tree peony | |
| KR20120139690A (en) | Liquid/liquid extraction | |
| JP7042764B2 (en) | Tomato extract and its manufacturing method, as well as foods and drinks and cosmetics containing tomato extract | |
| CN113683490B (en) | Preparation method of hypocannabidiol crystal | |
| CN105693683A (en) | A method of removing a plasticiser from vitamin E | |
| Singleton et al. | A method for adsorbent fractionation of cottonseed oil for experimental intravenous fat emulsions | |
| JPH0873396A (en) | Lipid having high natural menaquinone-7 content | |
| JP3651935B2 (en) | How to recover carotene | |
| Lee et al. | Heptadecanols from the leaves of Persea americana var. americana | |
| JPH0948969A (en) | Antioxidizing substance derived from citrus fruit | |
| CA2628304C (en) | Method of refining episesamin | |
| CN1810785A (en) | Prepn of lutein fally ester and lutein | |
| JP3944532B2 (en) | Method for producing high purity β-cryptoxanthin | |
| JP2017019756A (en) | Tomato extract and its producing method, and food and drink and cosmetic including tomato extract | |
| KR101049206B1 (en) | Preparation method of fat-soluble tea polyphenol | |
| Minh | Parameters affecting oil extraction from rambutan (Nephelium lappaceum L.) seed | |
| CN107056605A (en) | The method that unrighted acid and phytosterol are separated from Ghana's seed grease |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |