CN101654447A - Extraction method of natural vitamin E - Google Patents
Extraction method of natural vitamin E Download PDFInfo
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- CN101654447A CN101654447A CN200910192486A CN200910192486A CN101654447A CN 101654447 A CN101654447 A CN 101654447A CN 200910192486 A CN200910192486 A CN 200910192486A CN 200910192486 A CN200910192486 A CN 200910192486A CN 101654447 A CN101654447 A CN 101654447A
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- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 title abstract description 156
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 title abstract description 77
- 229930003427 Vitamin E Natural products 0.000 title abstract description 76
- 239000011709 vitamin E Substances 0.000 title abstract description 76
- 235000019165 vitamin E Nutrition 0.000 title abstract description 76
- 229940046009 vitamin E Drugs 0.000 title abstract description 76
- 238000000605 extraction Methods 0.000 title abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 38
- 238000000926 separation method Methods 0.000 claims abstract description 31
- 238000004440 column chromatography Methods 0.000 claims abstract description 30
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 claims abstract description 14
- 238000010521 absorption reaction Methods 0.000 claims abstract description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 5
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- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 5
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- 239000001569 carbon dioxide Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000000470 constituent Substances 0.000 claims description 7
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- 239000000284 extract Substances 0.000 claims description 2
- 238000000746 purification Methods 0.000 abstract description 13
- 238000010924 continuous production Methods 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 239000000945 filler Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 42
- 238000005516 engineering process Methods 0.000 description 15
- 229930182558 Sterol Natural products 0.000 description 8
- 238000011084 recovery Methods 0.000 description 8
- 150000003432 sterols Chemical class 0.000 description 8
- 235000003702 sterols Nutrition 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 239000010685 fatty oil Substances 0.000 description 7
- 238000002955 isolation Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
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- GVJHHUAWPYXKBD-IEOSBIPESA-N α-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-IEOSBIPESA-N 0.000 description 5
- 230000004071 biological effect Effects 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 238000000199 molecular distillation Methods 0.000 description 3
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- 239000011732 tocopherol Substances 0.000 description 3
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- GJJVAFUKOBZPCB-ZGRPYONQSA-N (r)-3,4-dihydro-2-methyl-2-(4,8,12-trimethyl-3,7,11-tridecatrienyl)-2h-1-benzopyran-6-ol Chemical class OC1=CC=C2OC(CC/C=C(C)/CC/C=C(C)/CCC=C(C)C)(C)CCC2=C1 GJJVAFUKOBZPCB-ZGRPYONQSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
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- 229930014626 natural product Natural products 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 238000000194 supercritical-fluid extraction Methods 0.000 description 2
- 229940068778 tocotrienols Drugs 0.000 description 2
- 229940088594 vitamin Drugs 0.000 description 2
- 229930003231 vitamin Natural products 0.000 description 2
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- 150000003722 vitamin derivatives Chemical class 0.000 description 2
- GJJVAFUKOBZPCB-UHFFFAOYSA-N 2-methyl-2-(4,8,12-trimethyltrideca-3,7,11-trienyl)-3,4-dihydrochromen-6-ol Chemical compound OC1=CC=C2OC(CCC=C(C)CCC=C(C)CCC=C(C)C)(C)CCC2=C1 GJJVAFUKOBZPCB-UHFFFAOYSA-N 0.000 description 1
- 206010006187 Breast cancer Diseases 0.000 description 1
- 208000026310 Breast neoplasm Diseases 0.000 description 1
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- 235000001815 DL-alpha-tocopherol Nutrition 0.000 description 1
- 239000011627 DL-alpha-tocopherol Substances 0.000 description 1
- 229940087168 alpha tocopherol Drugs 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000002605 anti-dotal effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 235000010382 gamma-tocopherol Nutrition 0.000 description 1
- 230000002068 genetic effect Effects 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000003053 immunization Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
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- 210000000056 organ Anatomy 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 238000010898 silica gel chromatography Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 229960000984 tocofersolan Drugs 0.000 description 1
- 235000004835 α-tocopherol Nutrition 0.000 description 1
- 239000002076 α-tocopherol Substances 0.000 description 1
- 239000002478 γ-tocopherol Substances 0.000 description 1
- QUEDXNHFTDJVIY-DQCZWYHMSA-N γ-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1 QUEDXNHFTDJVIY-DQCZWYHMSA-N 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention discloses an extraction method of a natural vitamin E, which combines supercritical carbon dioxide extraction and column chromatography separation to extract the natural vitamin E, wherein the pressure of the column chromatography separation is 7 MPa-45 MPa, the temperature of the column chromatography separation is 31 DEG C-80 DEG C, and absorption fillers used for the column chromatography separation are active carbon and silica gel or aluminium oxide. The extraction method integrates a supercritical carbon dioxide extraction technique and a column chromatography separation technique, combines the respective advantages of the supercritical carbon dioxide extraction technique and the column chromatography separation technique, mutually makes up the respective shortages of the techniques; and the extraction method not only makes up the shortage of the low purity of a product obtained by the purification of the supercritical carbon dioxide extraction technique and but alsomakes up the shortages of the low yield and efficiency and the like of the column chromatography separation technique and also uses the advantages of the high efficiency and the easy continuous production realization of the supercritical carbon dioxide extraction technique and the high purity of the natural vitamin E obtained by the column chromatography separation technique.
Description
Technical field
The present invention relates to the extracting vitamin E technology, specifically, relate to a kind of extracting vitamin E method.
Background technology
Vitamin-E (VE) has another name called tocopherol, is one of VITAMIN of needed by human.It comprises α, β, γ, δ type tocopherol and corresponding tocotrienols 8 kinds of materials such as (tocotrienol), has the removing free radical, anticancer, anti-cardiovascular disease, raising immunizing power and antidotal effect.There are synthetic and natural product two big classes in the source of vitamin-E.Natural VE is the dextrorotatory form with physiologically active, i.e. the d type; And the synthetic product are raceme, i.e. the mixture of d type and l type, so the biological activity of natural VE is more than 2 times of synthetics, and the bio-absorbable degree is also high and have a better edible safety than synthetics.The biological activity of 8 kinds of tocopherol homologues and functionally also there are differences, the biological activity of alpha-tocopherol is the strongest, and Gamma-Tocopherol can be removed excessive free radical in the body effectively, stops the infringement that they cause protein, peptide and various organ.Tocotrienols also helps to reduce the cholesterol level in the blood, and it has preventive and therapeutic effect to mammary cancer.Nearly 2 years researchists have confirmed that natural VE can also regulate cell signal and genetic expression.Vitamin-E extensively applies in healthcare products, pharmaceuticals, food or fodder additives and the makeup according to the difference of its purity, and highly purified natural VE is the first-selection of pharmaceuticals and healthcare products especially.
2000 so far, and the demand of vitamin-E is with the speed increment of 10%-15% in the world wide.Although the market value of synthetic vitamin-E is more much lower than natural product at present, along with people's health care consciousness strengthens, natural vitamin E product will replace synthetics gradually and have its vast market.In order to satisfy the growing demand of natural VE, numerous and confused newly-built natural VE production line of the main manufacturer of world's natural VE or expansion natural VE throughput.The production of the natural VE of China belongs to the starting stage, the manufacturer of especially highly purified vitamin-E still less, and the general technical level is not high, throughput (producing 100t and 200t per year does not wait) less than normal, the yield of product and purity not high (being lower than 70%) cause biological activity on the low side.This situation makes the demand of domestic natural vitamin E product and price all be in a disadvantageous position in the international market, and tracing it to its cause is that the isolation technique that adopted falls behind or do not pass a test.In order to change the production status of present China natural VE, cater to pharmaceuticals and the health-product market demand to high purity natural vitamin E and graded product, it is imperative to work out production cost natural VE separation purification method low, that be suitable for suitability for industrialized production.
Vitamin-E method of purification and technology comprise solvent extration, molecular distillation method, chromatography, supercritical carbon dioxide extraction method for refining, urea adduct method at present.Solvent extration is to utilize the different solubility of each component of raw material in solvent to separate, but need carry out repeatedly extraction treatment and consume a large amount of organic solvents and energy consumption, and product has residual solvent to exist and influences its quality, generally can be used as the pre-treatment step of purification; Molecular distillation method is vitamin-E purification techniques commonly used both at home and abroad at present, but the purity of product is generally not high, generally is lower than 80%, even the recovery rate of the high purity product that obtains is also very low, relative cost is higher; Chromatography can obtain highly purified vitamin products (more than 90%), but the output of general column chromatography is less, is not suitable for scale operation, and needs to handle a large amount of organic solvents, makes that the production cost of this technology is very high; The product purity that urea adduct method obtains is lower, can not be used for producing as the high purity purification techniques; The supercritical carbon dioxide extraction distillation technology is the development in recent years novel green isolation technique of getting up, by the control break pressure and temperature to change the solubleness of solute in supercritical co, utilize solubleness different between each material to reach purification to target substance, because the extraction temperature of supercritical co is not high, organic solvent-free, isolated with oxygen, so supercritical carbon dioxide extraction method is particularly suitable for the extraction separation of natural active matter, but this technology is applied in vitamin-E purification aspect, the purity that equally yet exists target product is not high, is difficult to obtain the shortcoming of high purity vitamin-E product.Integrate, the purification techniques of vitamin-E also all exists deficiency separately at present.
Delivered paper and patent application that some vitamin-Es are purified in recent years successively, Luan Lixia etc. have delivered the technical study (Chinese grain and oil journal first phase 100-103 in 2006 page or leaf) of molecular distillation technique purification natural VE; Zhang Lihua etc. have delivered silica gel column chromatography purifying natural vitamin-E (Food Additives Used in China third phase 105-109 in 2008 page or leaf); Zhang Qian etc. have delivered the experimental study (2008 the 7th phase 69-72 of oil engineering page or leaf) of solvent method purifying natural vitamin-E; Liu Yun etc. have delivered supercritical CO
2The optimised process research (Food Additives Used in China fourth phase 26-31 in 2005 page or leaf) of twin columns counter-current extraction concentrated natural vitamin E; Shi Bingjie etc. have delivered the experimental study (modern chemical industry third phase 59-61 in 2008 page or leaf) of continuous countercurrent supercritical extraction natural VE; Patent " technology of fractionally extracting natural VE by supercritical CO 2 fluid " (application number 02115535.6); Patent " method of supercritical extraction and concentrated natural vitamin E " (application number 00103260.7).At above-mentioned related work all is research paper and the patent of extracting concentrated natural vitamin E technology in recent years.Above-mentioned article and patent all are at method unfolded research separately, be confined to again in the deficiency separately, particularly aspect the preparation of high purity natural vitamin E, rarely have technology to reach, even the column chromatography chromatogram technology can not reach high-content (more than 95%), and purification efficiency is not high.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists, a kind of extracting method that can obtain high purity natural vitamin E is provided.
To achieve these goals, the present invention adopts following technical scheme:
A kind of extracting method of natural VE adopts supercritical carbon dioxide extraction to separate to unite with column chromatography and extracts.After utilizing supercritical co and continuously feeding low levels natural VE raw material is miscible, the present invention enters the purification that separates of carrying out component in the column chromatography separating still, the employing supercritical carbon dioxide fluid is a moving phase, utilize grease, sterol, wax and vitamin-E in supercritical co solubleness and each component in chromatographic column with the different purifications that separate that reach each component of sorbent material linkage force, simultaneously each component by supercritical co stripping chromatographic column after, through step-down, changing after the temperature in different separators the order according to the time collects successively, thereby obtain highly purified natural vitamin E product, and the carbonic acid gas reusable edible after separating totally simultaneously can obtain the byproduct sterol, fatty oil and wax component etc.
In the said extracted method, the isolating pressure of described column chromatography is 7MPa～45Mpa, and temperature is 31 ℃～80 ℃.
In the said extracted method, it is gac, silica gel or aluminium sesquioxide that described column chromatography is separated used absorption weighting agent.
In the said extracted method, specifically comprise the steps:
The natural VE raw material is placed head tank, in the continuous input system of high-pressure pump; Emit carbonic acid gas from gas cylinder and become liquid after high-pressure pump rises to predetermined pressure 7MPa～45MPa through condenser, through heat exchanger heats to 31 ℃～80 ℃ of preset temperatures, with the raw material of high-pressure pump P2 input miscible after, enter and carry out the effective constituent separation in the column chromatography separating still, effusive supercritical carbon dioxide fluid is through decompression and change temperature from the column chromatography separating still, enter in the parallel separator, parallel separator is used to collect natural VE and other components, the separating pressure of parallel separator is 5MPa～25MPa, and separation temperature is 15 ℃～75 ℃.
Compared with prior art, the present invention has following beneficial effect:
Integrated supercritical carbon dioxide extraction method of the present invention and column chromatography separation technology, combine supercritical carbon dioxide extraction and column chromatography technology advantage separately, remedied the deficiency of technology separately again mutually, both remedied the low deficiency of product purity that supercritical carbon dioxide extraction method is purified and obtained, it is low to have remedied column chromatography technology recovery rate again, the deficiency that efficient is not high has been brought into play supercritical carbon dioxide extraction simultaneously and efficiently and has easily been realized the higher advantage of natural VE purity that serialization production, column chromatography technology obtain.The present invention has realized continuously feeding, separates continuously, obtains high purity natural vitamin E (more than 95%) product once.Orange transparent, the superior product quality of gained natural vitamin E product feature, no solid substance, product purity height (more than 95%), organic solvent-free does not have that farming is residual, heavy metal free pollutes, and is convenient to carry out the recovery rate height of large-scale industrial production, product.
Technological operation of the present invention is simple, can realize continuous production, and carbonic acid gas can recycle, and has avoided the use of a large amount of organic solvents, to reducing cost and protecting environment that positive meaning is arranged.Simultaneously can obtain sterol, fatty oil and wax component or the like byproduct.
Description of drawings
Fig. 1 is the extraction separation schema of embodiment 1-5.
Embodiment
Embodiment 1
Throw in commercially available crude product natural VE (40%) raw material 50g among the head tank T, through high-pressure pump P2 at the uniform velocity in the input system.Emit carbonic acid gas from gas cylinder Q and become liquid after high-pressure pump P1 rises to predetermined pressure 7MPa through condenser H1, be heated to 31 ℃ of preset temperatures through heat exchanger H2, with the raw material of high-pressure pump P2 input miscible after, entering high-pressure column chromatographic separation still E1 carries out effective constituent with E2 and separates, E1 and E2 in parallel, in pretend with absorption weighting agent aluminum oxide, the changeable column chromatography separator that uses.Effusive from E1 and E2, as to be dissolved with heterogeneity supercritical carbon dioxide fluid is respectively through reducing valve 4 and 5, and change temperature, in separator S1 (separating pressure is 5MPa, and separation temperature is 15 ℃) and S2 (separating pressure is 5MPa, and separation temperature is 15 ℃), collect different components.S1 and S2 are in parallel, and the collector of temperature controllable is used for collecting the different in time products that come out from the high-pressure column chromatographic separator.Time segment can be collected the fatty oil in the material among the S1, sterol and wax component, collect highly purified natural vitamin E product among the S2, through S1 and CO 2 fluid after S2 separates pass through again separator S3 (separating pressure is 5MPa, and separation temperature is 15 ℃) further isolation of purified after in device, recycle behind the valve 6, under meter F metering, condenser H1 condensation.In S1, collect impurity substances 23.1g; Collect among the S2 and obtain orange transparent natural vitamin E product 13.5g, natural VE content 96.5%, yield 65.1%, natural vitamin E product purity that obtains and recovery rate all obviously want high than additive method.
Embodiment 2
Throw in commercially available crude product natural VE (40%) raw material 50g among the head tank T, through high-pressure pump P2 at the uniform velocity in the input system.Emit carbonic acid gas from gas cylinder Q and become liquid after high-pressure pump P1 rises to predetermined pressure 10MPa through condenser H1, be heated to 55 ℃ of preset temperatures through heat exchanger H2, with the raw material of high-pressure pump P2 input miscible after, entering high-pressure column chromatographic separation still E1 carries out effective constituent with E2 and separates, E1 and E2 in parallel, in pretend with absorption weighting agent silica gel, the changeable column chromatography separator that uses.Effusive from E1 and E2, as to be dissolved with heterogeneity supercritical carbon dioxide fluid is respectively through reducing valve 4 and 5, and change temperature, in separator S1 (separating pressure is 6MPa, and separation temperature is 45 ℃) and S2 (separating pressure is 6MPa, and separation temperature is 45 ℃), collect different components.S1 and S2 are in parallel, and the collector of temperature controllable is used for collecting the different in time products that come out from the high-pressure column chromatographic separator.Time segment can be collected the fatty oil in the material among the S1, sterol and wax component, collect highly purified natural vitamin E product among the S2, through S1 and CO 2 fluid after S2 separates pass through again separator S3 (separating pressure is 6MPa, and separation temperature is 45 ℃) further isolation of purified after in device, recycle behind the valve 6, under meter F metering, condenser H1 condensation.In S1, collect impurity substances 26.3g; Collect among the S2 and obtain orange transparent natural vitamin E product 15.9g, natural VE content 95.3%, yield 75.8%, natural vitamin E product purity that obtains and recovery rate all obviously want high than additive method.
Throw in commercially available crude product natural VE (40%) raw material 50g among the head tank T, through high-pressure pump P2 at the uniform velocity in the input system.Emit carbonic acid gas from gas cylinder Q and become liquid after high-pressure pump P1 rises to predetermined pressure 20MPa through condenser H1, be heated to 40 ℃ of preset temperatures through heat exchanger H2, with the raw material of high-pressure pump P2 input miscible after, entering high-pressure column chromatographic separation still E1 carries out effective constituent with E2 and separates, E1 and E2 in parallel, in pretend with absorption weighting agent gac, the changeable column chromatography separator that uses.Effusive from E1 and E2, as to be dissolved with heterogeneity supercritical carbon dioxide fluid is respectively through reducing valve 4 and 5, and change temperature, in separator S1 (separating pressure is 4MPa, and separation temperature is 55 ℃) and S2 (separating pressure is 4MPa, and separation temperature is 55 ℃), collect different components.S1 and S2 are in parallel, and the collector of temperature controllable is used for collecting the different in time products that come out from the high-pressure column chromatographic separator.Time segment can be collected the fatty oil in the material among the S1, sterol and wax component, collect highly purified natural vitamin E product among the S2, through S1 and CO 2 fluid after S2 separates pass through again separator S3 (separating pressure is 4MPa, and separation temperature is 55 ℃) further isolation of purified after in device, recycle behind the valve 6, under meter F metering, condenser H1 condensation.In S1, collect impurity substances 31.7g; Collect among the S2 and obtain orange transparent natural vitamin E product 16.8g, natural VE content 97.2%, yield 81.7%, natural vitamin E product purity that obtains and recovery rate all obviously want high than additive method.
Embodiment 4
Throw in commercially available crude product natural VE (40%) raw material 50g among the head tank T, through high-pressure pump P2 at the uniform velocity in the input system.Emit carbonic acid gas from gas cylinder Q and become liquid after high-pressure pump P1 rises to predetermined pressure 35MPa through condenser H1, be heated to 67 ℃ of preset temperatures through heat exchanger H2, with the raw material of high-pressure pump P2 input miscible after, entering high-pressure column chromatographic separation still E1 carries out effective constituent with E2 and separates, E1 and E2 in parallel, in pretend with absorption weighting agent aluminum oxide, the changeable column chromatography separator that uses.Effusive from E1 and E2, as to be dissolved with heterogeneity supercritical carbon dioxide fluid is respectively through reducing valve 4 and 5, and change temperature, in separator S1 (separating pressure is 12MPa, and separation temperature is 60 ℃) and S2 (separating pressure is 12MPa, and separation temperature is 60 ℃), collect different components.S1 and S2 are in parallel, and the collector of temperature controllable is used for collecting the different in time products that come out from the high-pressure column chromatographic separator.Time segment can be collected the fatty oil in the material among the S1, sterol and wax component, collect highly purified natural vitamin E product among the S2, through S1 and CO 2 fluid after S2 separates pass through again separator S3 (separating pressure is 12MPa, and separation temperature is 60 ℃) further isolation of purified after in device, recycle behind the valve 6, under meter F metering, condenser H1 condensation.In S1, collect impurity substances 33.1g; Collect among the S2 and obtain orange transparent natural vitamin E product 12.8g, natural VE content 95.8%, yield 61.3%, natural vitamin E product purity that obtains and recovery rate all obviously want high than additive method.
Throw in commercially available crude product natural VE (40%) raw material 50g among the head tank T, through high-pressure pump P2 at the uniform velocity in the input system.Emit carbonic acid gas from gas cylinder Q and become liquid after high-pressure pump P1 rises to predetermined pressure 45MPa through condenser H1, be heated to 80 ℃ of preset temperatures through heat exchanger H2, with the raw material of high-pressure pump P2 input miscible after, entering high-pressure column chromatographic separation still E1 carries out effective constituent with E2 and separates, E1 and E2 in parallel, in pretend with absorption weighting agent silica gel, the changeable column chromatography separator that uses.Effusive from E1 and E2, as to be dissolved with heterogeneity supercritical carbon dioxide fluid is respectively through reducing valve 4 and 5, and change temperature, in separator S1 (separating pressure is 25MPa, and separation temperature is 75 ℃) and S2 (separating pressure is 25MPa, and separation temperature is 75 ℃), collect different components.S1 and S2 are in parallel, and the collector of temperature controllable is used for collecting the different in time products that come out from the high-pressure column chromatographic separator.Time segment can be collected the fatty oil in the material among the S1, sterol and wax component, collect highly purified natural vitamin E product among the S2, through S1 and CO 2 fluid after S2 separates pass through again separator S3 (separating pressure is 25MPa, and separation temperature is 75 ℃) further isolation of purified after in device, recycle behind the valve 6, under meter F metering, condenser H1 condensation.In S1, collect impurity substances 25.5g; Collect among the S2 and obtain orange transparent natural vitamin E product 12.3g, natural VE content 95.2%, yield 58.5%, natural vitamin E product purity that obtains and recovery rate all obviously want high than additive method.Described separator S1, S2 and S3 are meant that the change that utilizes the substance dissolves degree carries out isolating separator.
Claims (4)
1, a kind of extracting method of natural VE is characterized in that adopting supercritical carbon dioxide extraction to separate to unite with column chromatography and extracts.
2, extracting method as claimed in claim 1 is characterized in that the isolating pressure of described column chromatography is 7MPa～45MPa, and temperature is 31 ℃～80 ℃.
3, extracting method as claimed in claim 1 is characterized in that it is gac, silica gel or aluminium sesquioxide that described column chromatography is separated used absorption weighting agent.
4, extracting method as claimed in claim 1 is characterized in that comprising the steps:
The natural VE raw material is placed head tank, in the continuous input system of high-pressure pump; Emit carbonic acid gas from gas cylinder and become liquid after high-pressure pump rises to predetermined pressure 7MPa～45MPa through condenser, through heat exchanger heats to 31 ℃～80 ℃ of preset temperatures, with the raw material of high-pressure pump P2 input miscible after, enter and carry out the effective constituent separation in the column chromatography separating still, effusive supercritical carbon dioxide fluid is through decompression and change temperature from the column chromatography separating still, enter in the parallel separator, parallel separator is used to collect natural VE and other components, the separating pressure of parallel separator is 5MPa～25MPa, and separation temperature is 15 ℃～75 ℃.
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| CN200910192486A CN101654447B (en) | 2009-09-18 | 2009-09-18 | Extraction method of natural vitamin E |
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| CN200910192486A CN101654447B (en) | 2009-09-18 | 2009-09-18 | Extraction method of natural vitamin E |
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| CN101654447B CN101654447B (en) | 2012-10-03 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103399100A (en) * | 2013-08-13 | 2013-11-20 | 中国热带农业科学院农产品加工研究所 | Measuring method of vitamin E content in fruits |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103399100A (en) * | 2013-08-13 | 2013-11-20 | 中国热带农业科学院农产品加工研究所 | Measuring method of vitamin E content in fruits |
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