CN104262315A - Method for separating and purifying tocotrienols - Google Patents
Method for separating and purifying tocotrienols Download PDFInfo
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- CN104262315A CN104262315A CN201410453257.2A CN201410453257A CN104262315A CN 104262315 A CN104262315 A CN 104262315A CN 201410453257 A CN201410453257 A CN 201410453257A CN 104262315 A CN104262315 A CN 104262315A
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- China
- Prior art keywords
- polar solvent
- tocotrienols
- silica gel
- separating
- silver nitrate
- 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.)
- Pending
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- 235000019148 tocotrienols Nutrition 0.000 title claims abstract description 42
- 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 title claims abstract description 41
- 229930003802 tocotrienol Natural products 0.000 title claims abstract description 41
- 239000011731 tocotrienol Substances 0.000 title claims abstract description 41
- 229940068778 tocotrienols Drugs 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 28
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical group [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 42
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000741 silica gel Substances 0.000 claims abstract description 28
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 28
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000004440 column chromatography Methods 0.000 claims abstract description 9
- 239000000945 filler Substances 0.000 claims abstract description 9
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 7
- 239000003480 eluent Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001514 detection method Methods 0.000 claims abstract description 4
- 239000012141 concentrate Substances 0.000 claims abstract description 3
- 239000012454 non-polar solvent Substances 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 15
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 7
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000002798 polar solvent Substances 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- 238000004807 desolvation Methods 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 2
- 238000000199 molecular distillation Methods 0.000 claims description 2
- 238000010828 elution Methods 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 abstract 1
- 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 14
- 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 description 10
- 239000011732 tocopherol Substances 0.000 description 8
- 229930003799 tocopherol Natural products 0.000 description 8
- 235000010384 tocopherol Nutrition 0.000 description 7
- 229960001295 tocopherol Drugs 0.000 description 7
- 229960000984 tocofersolan Drugs 0.000 description 4
- 235000004835 α-tocopherol Nutrition 0.000 description 4
- 239000002076 α-tocopherol Substances 0.000 description 4
- 229940087168 alpha tocopherol Drugs 0.000 description 3
- OAYLNYINCPYISS-UHFFFAOYSA-N ethyl acetate;hexane Chemical compound CCCCCC.CCOC(C)=O OAYLNYINCPYISS-UHFFFAOYSA-N 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007127 saponification reaction Methods 0.000 description 2
- YYGNTYWPHWGJRM-UHFFFAOYSA-N (6E,10E,14E,18E)-2,6,10,15,19,23-hexamethyltetracosa-2,6,10,14,18,22-hexaene Chemical compound CC(C)=CCCC(C)=CCCC(C)=CCCC=C(C)CCC=C(C)CCC=C(C)C YYGNTYWPHWGJRM-UHFFFAOYSA-N 0.000 description 1
- 241000233788 Arecaceae Species 0.000 description 1
- ACTIUHUUMQJHFO-UHFFFAOYSA-N Coenzym Q10 Natural products COC1=C(OC)C(=O)C(CC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)C)=C(C)C1=O ACTIUHUUMQJHFO-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000209510 Liliopsida Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 241000209504 Poaceae Species 0.000 description 1
- 241000269319 Squalius cephalus Species 0.000 description 1
- BHEOSNUKNHRBNM-UHFFFAOYSA-N Tetramethylsqualene Natural products CC(=C)C(C)CCC(=C)C(C)CCC(C)=CCCC=C(C)CCC(C)C(=C)CCC(C)C(C)=C BHEOSNUKNHRBNM-UHFFFAOYSA-N 0.000 description 1
- 229930003427 Vitamin E Natural products 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 235000021466 carotenoid Nutrition 0.000 description 1
- 150000001747 carotenoids Chemical class 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 235000017471 coenzyme Q10 Nutrition 0.000 description 1
- ACTIUHUUMQJHFO-UPTCCGCDSA-N coenzyme Q10 Chemical compound COC1=C(OC)C(=O)C(C\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CCC=C(C)C)=C(C)C1=O ACTIUHUUMQJHFO-UPTCCGCDSA-N 0.000 description 1
- 229940110767 coenzyme Q10 Drugs 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- PRAKJMSDJKAYCZ-UHFFFAOYSA-N dodecahydrosqualene Natural products CC(C)CCCC(C)CCCC(C)CCCCC(C)CCCC(C)CCCC(C)C PRAKJMSDJKAYCZ-UHFFFAOYSA-N 0.000 description 1
- 241001233957 eudicotyledons Species 0.000 description 1
- 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 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000002378 plant sterols Nutrition 0.000 description 1
- 238000004262 preparative liquid chromatography Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229940031439 squalene Drugs 0.000 description 1
- TUHBEKDERLKLEC-UHFFFAOYSA-N squalene Natural products CC(=CCCC(=CCCC(=CCCC=C(/C)CCC=C(/C)CC=C(C)C)C)C)C TUHBEKDERLKLEC-UHFFFAOYSA-N 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 125000002640 tocopherol group Chemical class 0.000 description 1
- 235000019149 tocopherols Nutrition 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 239000011709 vitamin E Substances 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/70—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with two hydrocarbon radicals attached in position 2 and elements other than carbon and hydrogen in position 6
- C07D311/72—3,4-Dihydro derivatives having in position 2 at least one methyl radical and in position 6 one oxygen atom, e.g. tocopherols
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
- B01D15/206—Packing or coating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Pyrane Compounds (AREA)
Abstract
The invention discloses a method for separating and purifying tocotrienols. The method comprises the following steps: (1) preparing filler for chromatography; (2) carrying out column chromatography; and (3) fractionally collecting eluent, combining the eluent with same components according to TLC detection and carrying out concentration to obtain tocotrienols concentrate, wherein the filler for column chromatography is silver nitrate silica gel, in the preparation process of the silver nitrate silica gel, the proportion of the silver nitrate to the silica gel, the proportion of the added water to the ethyl alcohol and the parameters such as the column amount of the column chromatography and the drying time are adjusted, and a plurality of solvent systems are used for sequential elution, so that the elution of the active constituents are more complete and the yield of the tocotrienols is greatly improved. The method is simple in process, low in equipment requirement and high in separation efficiency.
Description
Technical field
The invention belongs to field of chemical engineering, be specifically related to a kind of separating and purifying method of tocotrienols.
Background technology
Vitamin-E is the general name of tocopherol and tocotrienols and the derivative (as ester class etc.) with d-alpha-tocopherol physiologically active.From plant resources, 4 kinds of tocopherols (α, β, γ, δ) and 4 kinds of tocotrienolss (α, β, γ, δ) are isolated at present.Tocotrienols and the structural key distinction of tocopherol are that isoprenoid base side chain degree of saturation is different.Why tocotrienols has carried no weight two reasons: one is in various tocopherol and tocotrienols, and the physiologically active of alpha-tocopherol is the highest, preferentially absorbed and utilize, and the physiologically active of tocotrienols is relatively low in human body; Two is that the distribution of tocotrienols is wide, only exist with monocotyledons (Gramineae and Palmae) and minority dicotyledons in find.
At present, the extraction purification research report about tocotrienols is little, and the difficulty of its extraction and isolation is: easily oxidational losses; Tocopherol and tocotrienols structure and character close, not easily separated.Its purification technique comprises: saponification is to remove the Ester in vegetables oil, but saponification reaction needs comparatively high temps and carries out in the basic conditions, the very easily oxidized loss of tocotrienols, therefore needs to add antioxidant; Supercritical CO
2extraction, the method effectively can overcome the shortcomings such as oxidizable, the dissolvent residual in tocotrienols sepn process, but required equipment cost is higher; Column chromatography chromatogram is separated can carry out roughing out to tocopherol and tocotrienols, makes most of tocopherol and tocotrienols carry out enrichment, but tocopherol cannot be made effectively to be separated with tocotrienols; Preparative liquid chromatography can obtain highly purified tocotrienols, but the method cost is high, equipment requirements is high, output is little, is not suitable for industrialization.
Summary of the invention
In order to overcome the deficiency of above-mentioned prior art, the invention provides a kind of separating and purifying method of tocotrienols, the method technique is simple, equipment requirements is low, separation efficiency is high.
The technical solution adopted in the present invention is, a kind of separating and purifying method of tocotrienols, specifically comprises the following steps:
(1) prepared by chromatography filler: in silica gel: the ratio mixing of Silver Nitrate=2.5 ~ 3.5:1 (m/m), add silica gel quality 1:1 ~ 2 (m/v) distilled water and 1:1.5 ~ 3 (m/v) ethanol, be uniformly mixed, underpressure distillation desolvation, the sample powder that must flow dries 16 ~ 24h in 100-120 DEG C;
(2) column chromatography: adopt wet method dress post, chromatography column is proceeded to by disposable after the immersion of Silver Nitrate silica gel non-polar solvent, with described non-polar solvent as eluent repeatedly wash-out filler make Silver Nitrate silica gel deposit compacting, by the upper column quantity of Silver Nitrate silica gel quality 5% ~ 30%, sample is transferred to silica gel top, then 0.5-1BV (column volume) non-polar solvent is pressed, the mixing elutriant of 0.5-1BV (column volume) 5% ~ 10% polar solvent-non-polar solvent, the sequentially eluting sample of the mixing elutriant of 0.5-1BV (column volume) 50% ~ 100% polar solvent-non-polar solvent,
(3) Fractional Collections elutriant, according to TLC combining data detection same composition elutriant, obtains tocotrienols concentrated solution after concentrated.
Preferably, in step (1), in silica gel: the ratio mixing of Silver Nitrate=2.5:1 (m/m).
Preferably, the non-polar solvent in step (2) is normal hexane, normal heptane or sherwood oil.
Preferably, the polar solvent in step (2) is ethyl acetate, tetrahydrofuran (THF) or chloroform.
Preferably, the non-polar solvent in step (2) is normal hexane, and polar solvent is ethyl acetate.
Preferably, by the upper column quantity of Silver Nitrate silica gel quality 5%, sample is transferred to silica gel top in step (2).
Preferably, the mixing elutriant of the polar solvent-non-polar solvent in step (2) is ethyl acetate-hexane.
Preferably, in step (2), by the sequentially eluting sample of the mixing elutriant of 1BV (column volume) non-polar solvent, 1BV (column volume) 10% polar solvent-non-polar solvent, the mixing elutriant of 1BV (column volume) 50% polar solvent-non-polar solvent.
Preferably, the simmer down to molecular distillation in step (3) concentrates.
The sample source that the present invention is separated is extensive, both plam oil and Rice pollard oil can be derived from, also can derive from the tankage of cereal processing and contain than more rich tocotrienols, the sample to be separated containing certain density tocotrienols is all suitable for method of the present invention.Sample source also can be obtained by purchase, the tocotrienols raw material produced as Malaysian Carotech company (wherein mixes tocotrienols content 25.32%, alpha-tocopherol content 6.9%, comprises squalene, plant sterol, Coenzyme Q10 99.0 and mixed type carotenoid etc. containing other compositions in addition).
Compared to existing technology, the present invention has following advantage:
1, column chromatography filler adopts Silver Nitrate silica gel, in the preparation process of Silver Nitrate silica gel, comprising the parameter such as ratio and drying time of Silver Nitrate and silica gel ratio, the water added and ethanol, is all the optimum proportioning that applicant gropes out through long-term creative work; The use successively of the upper column quantity that column chromatography adopts and multi-solvents system, namely the mixing elution of the polar solvent-non-polar solvent increased from non-polar solvent to concentration is adopted, make the wash-out of active principle more complete, greatly improve the yield of tocotrienols;
2, method technique of the present invention is simple, equipment requirements is low, separation efficiency is high, is suitable for industrialization.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
(1) prepared by chromatography filler: get silica gel 100g, Silver Nitrate 40g, adds 100ml distilled water and 150ml ethanol, is uniformly mixed, underpressure distillation desolvation, and the sample powder that must flow dries 20h in 120 DEG C;
(2) column chromatography: adopt wet method dress post, chromatography column is proceeded to by disposable after the immersion of Silver Nitrate silica gel normal hexane, with normal hexane as eluent repeatedly wash-out filler make Silver Nitrate silica gel deposit compacting, get 7g sample and be transferred to silica gel top, then press the eluent sequentially eluting sample of normal hexane 1BV, 10% ethyl acetate-hexane 1BV, 50% ethyl acetate-hexane 1BV; Sample source is obtained by purchase, the tocotrienols raw material (wherein mixing tocotrienols content 25.32%, alpha-tocopherol content 6.9%) that Malaysian Carotech company produces;
(3) Fractional Collections elutriant, according to TLC combining data detection same composition elutriant, obtains tocotrienols concentrated solution 1.99g, wherein tocotrienols content 85.57%, yield 81.0% after concentrated.
Above embodiment display and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; instead of limit the scope of the invention by any way; without departing from the scope of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in claimed scope.
Claims (8)
1. a separating and purifying method for tocotrienols, specifically comprises the following steps:
(1) prepared by chromatography filler: in silica gel: the ratio mixing of Silver Nitrate=2.5 ~ 3.5:1 (m/m), add silica gel quality 1:1 ~ 2 (m/v) distilled water and 1:1.5 ~ 3 (m/v) ethanol, be uniformly mixed, underpressure distillation desolvation, the sample powder that must flow dries 16 ~ 24h in 100-120 DEG C;
(2) column chromatography: adopt wet method dress post, chromatography column is proceeded to by disposable after the immersion of Silver Nitrate silica gel non-polar solvent, with described non-polar solvent as eluent repeatedly wash-out filler make Silver Nitrate silica gel deposit compacting, by the upper column quantity of Silver Nitrate silica gel quality 5% ~ 30%, sample is transferred to silica gel top, then 0.5-1BV (column volume) non-polar solvent is pressed, the mixing elutriant of 0.5-1BV (column volume) 5% ~ 10% polar solvent-non-polar solvent, the sequentially eluting sample of the mixing elutriant of 0.5-1BV (column volume) 50% ~ 100% polar solvent-non-polar solvent,
(3) Fractional Collections elutriant, according to TLC combining data detection same composition elutriant, obtains tocotrienols concentrated solution after concentrated.
2. the separating and purifying method of a kind of tocotrienols according to claim 1, is characterized in that, in step (1), in silica gel: the ratio mixing of Silver Nitrate=2.5:1 (m/m).
3. the separating and purifying method of a kind of tocotrienols according to claim 1, is characterized in that, the non-polar solvent in step (2) is normal hexane, normal heptane or sherwood oil.
4. the separating and purifying method of a kind of tocotrienols according to claim 1, is characterized in that, the polar solvent in step (2) is ethyl acetate, tetrahydrofuran (THF) or chloroform.
5. the separating and purifying method of a kind of tocotrienols according to claim 1, is characterized in that, the non-polar solvent in step (2) is normal hexane, and polar solvent is ethyl acetate.
6. the separating and purifying method of a kind of tocotrienols according to claim 1, is characterized in that, by the upper column quantity of Silver Nitrate silica gel quality 5%, sample is transferred to silica gel top in step (2).
7. the separating and purifying method of a kind of tocotrienols according to claim 1, it is characterized in that, in step (2), by the sequentially eluting sample of the mixing elutriant of 1BV (column volume) non-polar solvent, 1BV (column volume) 10% polar solvent-non-polar solvent, the mixing elutriant of 1BV (column volume) 50% polar solvent-non-polar solvent.
8. the separating and purifying method of a kind of tocotrienols according to claim 1, is characterized in that, the simmer down to molecular distillation in step (3) concentrates.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410453257.2A CN104262315A (en) | 2014-09-05 | 2014-09-05 | Method for separating and purifying tocotrienols |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410453257.2A CN104262315A (en) | 2014-09-05 | 2014-09-05 | Method for separating and purifying tocotrienols |
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| CN104262315A true CN104262315A (en) | 2015-01-07 |
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| CN201410453257.2A Pending CN104262315A (en) | 2014-09-05 | 2014-09-05 | Method for separating and purifying tocotrienols |
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|---|---|---|---|---|
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2014
- 2014-09-05 CN CN201410453257.2A patent/CN104262315A/en active Pending
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