CN101879436A - Decolorizing column and method for decolorizing DHA (docosahexaenoic acid) grease at normal temperature by using same - Google Patents
Decolorizing column and method for decolorizing DHA (docosahexaenoic acid) grease at normal temperature by using same Download PDFInfo
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- CN101879436A CN101879436A CN201010227935.5A CN201010227935A CN101879436A CN 101879436 A CN101879436 A CN 101879436A CN 201010227935 A CN201010227935 A CN 201010227935A CN 101879436 A CN101879436 A CN 101879436A
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- 239000004519 grease Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 31
- MBMBGCFOFBJSGT-KUBAVDMBSA-N all-cis-docosa-4,7,10,13,16,19-hexaenoic acid Chemical compound CC\C=C/C\C=C/C\C=C/C\C=C/C\C=C/C\C=C/CCC(O)=O MBMBGCFOFBJSGT-KUBAVDMBSA-N 0.000 title description 48
- 235000020669 docosahexaenoic acid Nutrition 0.000 title description 45
- 229940090949 docosahexaenoic acid Drugs 0.000 title description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 130
- 239000000203 mixture Substances 0.000 claims abstract description 56
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 48
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims abstract description 35
- 229930006000 Sucrose Natural products 0.000 claims abstract description 35
- 239000005720 sucrose Substances 0.000 claims abstract description 35
- 150000002978 peroxides Chemical class 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 88
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 54
- 229910052799 carbon Inorganic materials 0.000 claims description 38
- 239000003480 eluent Substances 0.000 claims description 26
- 239000000741 silica gel Substances 0.000 claims description 21
- 229910002027 silica gel Inorganic materials 0.000 claims description 21
- 238000009874 alkali refining Methods 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000002845 discoloration Methods 0.000 claims description 9
- 238000011049 filling Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 230000008030 elimination Effects 0.000 claims description 6
- 238000003379 elimination reaction Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000006210 lotion Substances 0.000 claims description 4
- 238000011084 recovery Methods 0.000 claims description 3
- 239000002253 acid Substances 0.000 abstract description 14
- 238000004332 deodorization Methods 0.000 abstract description 14
- 239000000194 fatty acid Substances 0.000 abstract description 7
- 239000000945 filler Substances 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 7
- 235000020777 polyunsaturated fatty acids Nutrition 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 235000014113 dietary fatty acids Nutrition 0.000 abstract 1
- 229930195729 fatty acid Natural products 0.000 abstract 1
- 150000004665 fatty acids Chemical class 0.000 abstract 1
- 239000012530 fluid Substances 0.000 abstract 1
- 229960001866 silicon dioxide Drugs 0.000 description 18
- 239000000341 volatile oil Substances 0.000 description 17
- 239000003921 oil Substances 0.000 description 13
- 239000000049 pigment Substances 0.000 description 12
- 230000003647 oxidation Effects 0.000 description 10
- 238000007254 oxidation reaction Methods 0.000 description 10
- 239000000796 flavoring agent Substances 0.000 description 8
- 125000001931 aliphatic group Chemical group 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 238000005056 compaction Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 241000195493 Cryptophyta Species 0.000 description 4
- 230000031700 light absorption Effects 0.000 description 4
- 235000019197 fats Nutrition 0.000 description 3
- 150000002432 hydroperoxides Chemical class 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000001877 deodorizing effect Effects 0.000 description 2
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 2
- 235000019634 flavors Nutrition 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 235000010358 acesulfame potassium Nutrition 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229940023032 activated charcoal Drugs 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 235000021466 carotenoid Nutrition 0.000 description 1
- 150000001747 carotenoids Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 208000029078 coronary artery disease Diseases 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000004438 eyesight Effects 0.000 description 1
- 230000035558 fertility Effects 0.000 description 1
- 210000003754 fetus Anatomy 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
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- 235000020978 long-chain polyunsaturated fatty acids Nutrition 0.000 description 1
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Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses a decoloring column, which is filled with activated silica gel, a mixture of diatomite 545 and activated carbon, a mixture of diatomite 545 and sucrose and activated silica gel from the bottom to the top of the column respectively; wherein the mass ratio of the four fillers is 0.5-2: 0.5-1.5: 0.5-2. The invention also discloses a preparation method of the decolorizing column and a normal-temperature decolorizing method for DHA grease by using the decolorizing column. The decoloring process of the invention is carried out at normal temperature; the decolored oil is nearly colorless, and the peroxide value, acid value and fishy smell are obviously reduced; the temperature and time of the subsequent deodorization process are reduced, the conversion of polyunsaturated fatty acid to trans-fatty acid at high temperature is avoided, and the energy consumption is saved; the loss of DHA grease is less, and the fatty acid composition is not obviously changed; the oil sample was clear and very fluid. Therefore, the method can improve the quality of the DHA grease.
Description
Technical field
The invention belongs to the bioseparation technology field, be specifically related to a kind of decolorizing column and utilize it to carry out the low temperature discoloration method of DHA grease.
Background technology
(Docosahexaenoic Acid is a kind of important n-3 long-chain polyunsaturated fatty acid DHA) to DHA, is commonly called as brain gold, has the memory of enhancing, improves intelligence, reduces blood fat, regulates effects such as immune system.DHA has the important physical effect to growing of infant, can promote fetus, infant's intelligence and eyesight to grow, and therefore adds DHA and more and more come into one's own in dispensed food for baby.The content that little algae produces polyunsaturated fatty acid in the DHA grease accounts for more than 70%, because it is rich in cis-double bonds, owing to long high temperature action, the cis-double bonds of unrighted acid can change into opposite form in decolouring and deodorising process, thereby the content of trans-fatty acid is increased.Trans-fatty acid is difficult to be caused physiological function multiple combination obstacle to occur easily by human consumption: reduce memory; Cause and get fat; Cause coronary heart disease; Influence is grown and male fecundity.Therefore to avoid DHA grease Long contact time at high temperature in DHA grease refining decolouring and deodorization link.It is high because of its degree of unsaturation that little algae produces the DHA grease, and easily oxidation produces off-flavors; To be rich in the carotenoid color and luster darker because of it again.In order to reduce color and luster and off-flavors, decoloration process is taked under the vacuum condition usually, and 100～120 ℃ decoloured 2～3 hours down, and this method can only partly reduce pigment, peroxide and the stench flavor in the grease.Most of pigment is still removed by the pyrolytic in the follow-up deodorization procedures, and pigment decomposition product and other stench flavor material are along with high-temperature water vapor heats up in a steamer then; Conventional deodorization condition is: 150～180 ℃, and high-temperature water vapor stripping deodorization 3～5 hours.This kind deodorizing technology energy consumption is big, length consuming time.
Summary of the invention
Technical problem to be solved by this invention provides a kind of decolorizing column, can be used for the normal temperature decolouring that little algae produces the DHA grease, reduced the temperature and time of follow-up deodorizing technology, avoided under the high temperature polyunsaturated fatty acid to the transformation of trans-fatty acid, and removed pigment, hydroperoxides and off-flavors effectively, improved the quality of DHA grease.
The technical problem that the present invention also will solve provides the preparation method of above-mentioned decolorizing column.
The technical problem that the present invention will solve at last provides utilizes above-mentioned decolorizing column to carry out the normal temperature discoloration method of DHA grease.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A kind of decolorizing column, this decolorizing column is from filling mixture, the activated silica gel of mixture, diatomite 545 and the sucrose of activated silica gel, diatomite 545 and active carbon respectively to capital at the bottom of the post; Wherein, activated silica gel, diatomite 545 are 0.5～2: 0.5～1.5 with mixture, the diatomite 545 of active carbon with the mixture of sucrose and the mass ratio of activated silica gel: 0.5～1.5: 0.5～2; In the mixture of diatomite 545 and active carbon, diatomite 545 is 1: 1～4 with the mass ratio of active carbon; In the mixture of diatomite 545 and sucrose, diatomite 545 is 1: 1～4 with the mass ratio of sucrose; The decolorizing column ratio of height to diameter is 10～20: 1.
Wherein, described silica gel is 100～400 orders; Described active carbon is 50～200 orders.
The preparation method of above-mentioned decolorizing column comprises the steps:
(1) silica gel is after methyl alcohol soaks, and suction filtration reclaims methyl alcohol, and with 3～5 times of deionized water rinsing silica gel to the methyl alcohol volume, heating activated and obtains activated silica gel in 12～15 hours under elimination moisture was placed on 100～110 ℃;
(2) diatomite 545 and active carbon are obtained the mixture of diatomite 545 and active carbon by mass ratio 1: 1～4 stirring and evenly mixings; Diatomite 545 and sucrose are obtained the mixture of diatomite 545 and sucrose by mass ratio 1: 1～4 stirring and evenly mixings;
(3) diatomite 545 that step (2) is obtained is immersed in respectively in the n-hexane with the mixture of the mixture of active carbon and diatomite 545 and sucrose, detects less than peroxide value (POV) until washing lotion with the n-hexane filter wash repeatedly;
(4) mixture of the mixture of activated silica gel, diatomite 545 and active carbon, diatomite 545 and sucrose, activated silica gel are by mass ratio 0.5～2: respectively be immersed in n-hexane in the middle of at 0.5～1.5: 0.5～1.5: 0.5～2; Adopt wet method to fill out post, from insert mixture, the activated silica gel of mixture, diatomite 545 and the sucrose of activated silica gel, diatomite 545 and active carbon at the bottom of the post successively to capital, the decolorizing column ratio of height to diameter is 10～20: 1;
(5) washing decolorizing column with n-hexane detects less than peroxide value (POV) until eluent.
In the step (4), pressurization 0.1～0.5Mpa when every layer material is inserted is so that filling compaction.
Utilize above-mentioned decolorizing column to carry out the normal temperature discoloration method of DHA grease, DHA grease behind the alkali refining is dissolved in the n-hexane by 1: 1～4 volume ratio, inject decolorizing column purity nitrogen pressurization wash-out or decompress filter, add n-hexane then and continue not contain in the straight eluent of wash-out grease (soon eluent drops in and do not have oil stain to show that eluent does not contain grease on the filter paper), collect eluent, obtain light DHA grease behind the recovery n-hexane.
Wherein, the pressure condition of pressurization wash-out is 0.1～0.5Mpa.
Wherein, the pressure condition of decompress filter be-0.05～-0.1Mpa.
Wherein, the condition of recovery n-hexane is-0.1Mpa 30～60 ℃ from eluent.
The light DHA grease that above-mentioned decoloration process obtains carries out the stripping deodorization through conventional technology, and temperature is 130～150 ℃, 30～60 minutes time, promptly gets the DHA essential oil.
It is because it has polarity as a kind of filler that the present invention adopts silica gel, and its microcellular structure is easy to adsorb polar compound in the grease such as free fatty, phosphatide, sweet one (two) ester, polarity pigment, Oxidation of Fat and Oils product etc.Characteristics such as selecting active carbon is big because of its specific area as filler, and adsorption rate is fast, adding itself is a kind of non-polar solid adsorbent, very easily adsorbs the little component of polarity in the grease, as nonpolar pigment, alkane, odoring substance etc.That diatomite 545 has is loose, porous, sorptive force and characteristics such as permeability is strong and particle is tiny, and it has adsorbent and two kinds of effects of filter aid concurrently in the present invention.Sucrose is tiny hard because of its crystalline particle, serves as filter aid in the present invention.Because adopt single silica gel to fill out post, lose shape because of the big elution speed of resistance slow, and can only the absorbed portion pigment; Adopt the single-activity charcoal to fill out post, resistance is big when walking post equally, and decolorizing effect is not obvious under the normal temperature, and small activated carbon granule is arranged and with special coke smell in the eluent.The present invention is provided with layer of silica gel at the chromatographic column capital and is to make the polar compound in the grease preferentially to be adsorbed; It down is provided with diatomite 545/ sucrose mixed layer again and is its filtrating aid function, the resistance when slowing down single silica gel and walking post; Lower floor is provided with diatomite 545/ active carbon mixed layer and is to adsorb weakly polar component in the grease again; The bottom is provided with once more that layer of silica gel is to adsorb the little component that does not eliminate and the material that stops activated carbon granule and have a coke smell enters in the final eluent, plays suction-operated again.
Beneficial effect: the present invention compared with prior art has following advantage:
1, the present invention provides a kind of multilayer filler of low temperature to analyse chromatography efficient decolorizing technology for little algae produces the DHA grease, the temperature and the deodorization time of follow-up deodorization procedures have been reduced, avoid the formation of trans-fatty acid, reduced energy consumption, and removed pigment, hydroperoxides and off-flavors effectively, improved the quality of DHA grease.
2, the present invention is based on activated silica gel, diatomite and active carbon have very strong adsorption capacity, at through coming unstuck and the DHA grease of alkali-refining process, adopt multilayer filler chromatographic column under normal temperature pressurization (or decompress filter), to carry out efficient adsorption bleaching, reduce hydroperoxides and off-flavors, reduce the time of staying of DHA grease in follow-up high temperature deodorization procedures, avoided the formation of trans-fatty acid in the high temperature decoloration and deodorization link.
The specific embodiment
According to following embodiment, the present invention may be better understood.Yet, those skilled in the art will readily understand that the described concrete material proportion of embodiment, process conditions and result thereof only are used to illustrate the present invention, and should also can not limit the present invention described in detail in claims.
Embodiment 1: the preparation of decolorizing column.
(1) 120g silica gel (gross porosity, 100～200 orders, Haiyang Chemical Plant, Qingdao) after 500mL methyl alcohol soaked 1 hour, suction filtration reclaimed methyl alcohol, with 4 times of deionized water rinsing silica gel to the methyl alcohol volume, heating activated more than 12 hours and obtains activated silica gel under elimination moisture was placed on 100～110 ℃;
(2) diatomite 545 and active carbon are obtained the mixture of diatomite 545 and active carbon (100 order) by 1: 2 stirring and evenly mixing of mass ratio; Diatomite 545 and sucrose are obtained the mixture of diatomite 545 and sucrose by 1: 2 stirring and evenly mixing of mass ratio;
(3) diatomite 545 that step (2) is obtained is immersed in respectively in the n-hexane with the mixture of the mixture of active carbon and diatomite 545 and sucrose, detects less than peroxide value (POV) until washing lotion with the n-hexane filter wash repeatedly;
(4) mixture, the 50g activated silica gel of the mixture of 50g activated silica gel, 50g diatomite 545 and active carbon, 50g diatomite 545 and sucrose is immersed in the middle of the n-hexane respectively; Adopt wet method to fill out post, select 4cm i.d * 60cm chromatographic column for use, from inserting the mixture, diatomite 545 of activated silica gel, diatomite 545 and active carbon and mixture, the activated silica gel of sucrose successively to capital at the bottom of the post, and wash post by pressurize (0.05Mpa) and make filling compaction.
(5) washing decolorizing column with n-hexane is 0 until the eluent peroxide value.
Embodiment 2: the preparation of decolorizing column.
(1) 120g silica gel (gross porosity, 100～200 orders, Haiyang Chemical Plant, Qingdao) after 500mL methyl alcohol soaked 1 hour, suction filtration reclaimed methyl alcohol, with 3 times of deionized water rinsing silica gel to the methyl alcohol volume, heating activated more than 12 hours and obtains activated silica gel under elimination moisture was placed on 100 ℃;
(2) diatomite 545 and active carbon are obtained the mixture of diatomite 545 and active carbon (200 order) by 1: 1 stirring and evenly mixing of mass ratio; Diatomite 545 and sucrose are obtained the mixture of diatomite 545 and sucrose by 1: 2 stirring and evenly mixing of mass ratio;
(3) diatomite 545 that step (2) is obtained is immersed in respectively in the n-hexane with the mixture of the mixture of active carbon and diatomite 545 and sucrose, detects less than peroxide value (POV) until washing lotion with the n-hexane filter wash repeatedly;
(4) mixture, the 60g activated silica gel of the mixture of 20g activated silica gel, 60g diatomite 545 and active carbon, 20g diatomite 545 and sucrose is immersed in the middle of the n-hexane respectively; Adopt wet method to fill out post, select 3.5cmi.d * 50cm chromatographic column for use, from inserting the mixture, diatomite 545 of activated silica gel, diatomite 545 and active carbon and mixture, the activated silica gel of sucrose successively to capital at the bottom of the post, and wash post by pressurize (0.05Mpa) and make filling compaction.
(5) washing decolorizing column with n-hexane is 0 until the eluent peroxide value.
Embodiment 3: the preparation of decolorizing column.
(1) 120g silica gel (gross porosity, 100～200 orders, Haiyang Chemical Plant, Qingdao) after 500mL methyl alcohol soaked 1 hour, suction filtration reclaimed methyl alcohol, with 3 times of deionized water rinsing silica gel to the methyl alcohol volume, heating activated more than 12 hours and obtains activated silica gel under elimination moisture was placed on 110 ℃;
(2) diatomite 545 and active carbon are obtained the mixture of diatomite 545 and active carbon (50 order) by 1: 1 stirring and evenly mixing of mass ratio; Diatomite 545 and sucrose are obtained the mixture of diatomite 545 and sucrose by 1: 2 stirring and evenly mixing of mass ratio;
(3) diatomite 545 that step (2) is obtained is immersed in respectively in the n-hexane with the mixture of the mixture of active carbon and diatomite 545 and sucrose, detects less than peroxide value (POV) until eluent with the n-hexane filter wash repeatedly;
(4) be immersed in the n-hexane with mixture, the 15g diatomite 545 of active carbon respectively with mixture, the 60g activated silica gel of sucrose 60g activated silica gel, 15g diatomite 545; Adopt wet method to fill out post, select 3.5cm i.d * 50cm chromatographic column for use, from inserting the mixture, diatomite 545 of activated silica gel, diatomite 545 and active carbon and mixture, the activated silica gel of sucrose successively to capital at the bottom of the post, and wash post by pressurize (0.05Mpa) and make filling compaction.
(5) washing decolorizing column with n-hexane is 0 until the eluent peroxide value.
The normal temperature decolouring of embodiment 4:DHA grease.
The volume ratio of DHA grease behind the 200g alkali refining by 1: 1 is dissolved in the n-hexane, inject decolorizing column purity nitrogen pressurization (0.1Mpa) wash-out that embodiment 1 makes, adding n-hexane then continues the straight eluent of wash-out and drops in and do not have oil stain on the filter paper, collect eluent, (0.1Mpa) rotation obtains light DHA grease after reclaiming n-hexane to 45 ℃ of following vacuum.Gained decolouring oil sample is under 130 ℃, and stripping deodorization 30 minutes promptly gets DHA essential oil 187g.The gained essential oil is measured its one-level oxidation index (POV), secondary oxidation index (TBARS), acid value, pigment light absorption value and is listed in table 1, and the aliphatic acid of gained essential oil is formed and listed in table 2.
The normal temperature decolouring of embodiment 5:DHA grease.
The volume ratio of DHA grease behind the 150g alkali refining by 1: 2 is dissolved in the n-hexane, the decolorizing column vacuum filtration that injection embodiment 2 makes (0.05～-0.1Mpa), adding n-hexane then continues the straight eluent of wash-out and drops in and do not have oil stain on the filter paper, collect eluent, (0.1Mpa) rotation obtains light DHA grease after reclaiming n-hexane to 55 ℃ of following vacuum.Gained decolouring oil sample is under 150 ℃, and stripping deodorization 30 minutes promptly gets DHA essential oil 141g.The gained essential oil is measured its one-level oxidation index (POV), secondary oxidation index (TBARS), acid value, pigment light absorption value and is listed in table 1, and the aliphatic acid of gained essential oil is formed and listed in table 2.
Comparative Examples 1:
200g silica gel (200 order) is after 500mL methyl alcohol soaks, and suction filtration reclaims methyl alcohol, and with 4 times of deionized water rinsing silica gel to the methyl alcohol volume, heating activated more than 12 hours and obtains activated silica gel under elimination moisture was placed on 100～110 ℃.Get the 200g activated silica gel and be immersed in the n-hexane, adopt wet method to fill out post, select 4cm i.d * 60cm chromatographic column for use, and wash post by pressurize (0.05Mpa) and make filling compaction.Washing post with n-hexane is 0 until the eluent peroxide value.
The volume ratio of DHA grease behind the 200g alkali refining by 1: 1 is dissolved in the n-hexane, inject above-mentioned silicagel column purity nitrogen pressurization (0.1Mpa) wash-out, adding n-hexane then continues the straight eluent of wash-out and drops in and do not have oil stain on the filter paper, collect eluent, (0.1Mpa) rotation obtains light DHA grease after reclaiming n-hexane to 45 ℃ of following vacuum.Gained decolouring oil sample is under 130 ℃, and stripping deodorization 30 minutes promptly gets DHA essential oil 183g.The gained essential oil is measured its one-level oxidation index (POV), secondary oxidation index (TBARS), acid value, pigment light absorption value and is listed in table 1, and the aliphatic acid of gained essential oil is formed and listed in table 2.The result shows that adopt single silica gel to fill out the post decolouring and compare with multilayer filler discoloration method: (1) can not reduce the POV and the TBARS of DHA grease fully; (2) decolorizing effect relatively a little less than; (3) gained DHA essential oil is compared with the aliphatic acid composition of alkali refining DHA grease, and the polyunsaturated fatty acid total content slightly rises.
Comparative Examples 2:
Get 200g active carbon (100 order) and be immersed in the n-hexane, adopt wet method to fill out post, select 4cm i.d * 60cm chromatographic column for use, and wash post by pressurize (0.05Mpa) and make filling compaction.Washing post with n-hexane is 0 until the eluent peroxide value.
The volume ratio of DHA grease behind the 200g alkali refining by 1: 1 is dissolved in the n-hexane, injects above-mentioned activated-charcoal column
The chemical property of table 1DHA essential oil and alkali refining oil
The aliphatic acid of table 2DHA essential oil and alkali refining oil is formed (area normalization method)
Purity nitrogen pressurization (0.1Mpa) wash-out adds n-hexane then and continues the straight eluent of wash-out and drop in and do not have oil stain on the filter paper, collects eluent, and (0.1Mpa) rotation obtains light DHA grease after reclaiming n-hexane to 45 ℃ of following vacuum.Gained decolouring oil sample is under 130 ℃, and stripping deodorization 30 minutes promptly gets DHA essential oil 172g.The gained essential oil is measured its one-level oxidation index (POV), secondary oxidation index (TBARS), acid value, pigment light absorption value and is listed in table 1, and the aliphatic acid of gained essential oil is formed and listed in table 2.The result shows that the single-activity charcoal is filled out the post decolouring and compared with the decolouring of multilayer filler: (1) can not reduce POV, TBARS and the acid value of DHA grease effectively, thereby oil sample still has off-flavors; (2) decolorizing effect is not obvious; (3) gained DHA essential oil is compared with the aliphatic acid composition of alkali refining DHA grease, and the polyunsaturated fatty acid total content slightly descends.
Claims (8)
1. a decolorizing column is characterized in that this decolorizing column is from filling mixture, the activated silica gel of mixture, diatomite 545 and the sucrose of activated silica gel, diatomite 545 and active carbon respectively to capital at the bottom of the post; Wherein, activated silica gel, diatomite 545 are 0.5～2: 0.5～1.5 with mixture, the diatomite 545 of active carbon with the mixture of sucrose and the mass ratio of activated silica gel: 0.5～1.5: 0.5～2; In the mixture of diatomite 545 and active carbon, diatomite 545 is 1: 1～4 with the mass ratio of active carbon; In the mixture of diatomite 545 and sucrose, diatomite 545 is 1: 1～4 with the mass ratio of sucrose; The decolorizing column ratio of height to diameter is 10～20: 1.
2. decolorizing column according to claim 1 is characterized in that described silica gel is 100～400 orders; Described active carbon is 50～200 orders.
3. the preparation method of the described decolorizing column of claim 1 is characterized in that this method comprises the steps:
(1) silica gel is after methyl alcohol soaks, and suction filtration reclaims methyl alcohol, and with 3～5 times of deionized water rinsing silica gel to the methyl alcohol volume, heating activated and obtains activated silica gel in 12～15 hours under elimination moisture was placed on 100～110 ℃;
(2) diatomite 545 and active carbon are obtained diatomite 545 and Mixture of Activated Carbon by mass ratio 1: 1～4 stirring and evenly mixings; Diatomite 545 and sucrose are obtained the mixture of diatomite 545 and sucrose by mass ratio 1: 1～4 stirring and evenly mixings;
(3) diatomite 545 that step (2) is obtained is immersed in respectively in the n-hexane with the mixture of the mixture of active carbon and diatomite 545 and sucrose, detects less than peroxide value until washing lotion with the n-hexane filter wash repeatedly;
(4) mixture of the mixture of activated silica gel, diatomite 545 and active carbon, diatomite 545 and sucrose, activated silica gel are by mass ratio 0.5～2: respectively be immersed in n-hexane in the middle of at 0.5～1.5: 0.5～1.5: 0.5～2; Adopt wet method to fill out post, from the bottom of the post to capital insert successively activated silica gel, diatomite 545 and active carbon mixture,, activated silica gel, the decolorizing column ratio of height to diameter is 10～20: 1;
(5) washing decolorizing column with n-hexane detects less than peroxide value until eluent.
4. the preparation method of decolorizing column according to claim 3 is characterized in that in the step (4), pressurization 0.1～0.5Mpa when every layer material is inserted.
5. utilize the described decolorizing column of claim 1 to carry out the normal temperature discoloration method of DHA grease, it is characterized in that the DHA grease behind the alkali refining is dissolved in the n-hexane by 1: 1～4 volume ratio, inject decolorizing column purity nitrogen pressurization wash-out or decompress filter, adding n-hexane then continues not contain grease in the straight eluent of wash-out, collect eluent, obtain light DHA grease behind the recovery n-hexane.
6. the normal temperature discoloration method that utilizes decolorizing column to carry out the DHA grease according to claim 5, the pressure condition of the wash-out that it is characterized in that pressurizeing is 0.1～0.5Mpa.
7. the normal temperature discoloration method that utilizes decolorizing column to carry out the DHA grease according to claim 5, the pressure condition that it is characterized in that decompress filter be-0.05～-0.1Mpa.
8. the normal temperature discoloration method that utilizes decolorizing column to carry out the DHA grease according to claim 5 is characterized in that the condition that reclaims n-hexane from eluent is-0.1Mpa 30～60 ℃.
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| CN103908946A (en) * | 2013-01-07 | 2014-07-09 | 丰益(上海)生物技术研发中心有限公司 | Mixed adsorbent, grease and preparation method thereof |
| CN104711118A (en) * | 2013-12-16 | 2015-06-17 | 丰益(上海)生物技术研发中心有限公司 | Method for reducing trans fatty acids |
| CN105218367A (en) * | 2014-06-09 | 2016-01-06 | 四川国为制药有限公司 | A kind of High Purity Ethyl Eicosapentaenoate enriched material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103908946A (en) * | 2013-01-07 | 2014-07-09 | 丰益(上海)生物技术研发中心有限公司 | Mixed adsorbent, grease and preparation method thereof |
| CN103908946B (en) * | 2013-01-07 | 2018-04-06 | 丰益(上海)生物技术研发中心有限公司 | A kind of mixed adsorbent, grease and preparation method thereof |
| CN104711118A (en) * | 2013-12-16 | 2015-06-17 | 丰益(上海)生物技术研发中心有限公司 | Method for reducing trans fatty acids |
| CN104711118B (en) * | 2013-12-16 | 2019-02-22 | 丰益(上海)生物技术研发中心有限公司 | A method of reducing trans-fatty acid |
| CN105218367A (en) * | 2014-06-09 | 2016-01-06 | 四川国为制药有限公司 | A kind of High Purity Ethyl Eicosapentaenoate enriched material |
| CN108802363A (en) * | 2018-06-13 | 2018-11-13 | 广东腾湃医疗股份有限公司 | A kind of novel purification cadmium chelating type immune complex method |
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Assignee: JIANGSU HENGSHUNDA BIO-ENERGY Co.,Ltd. Assignor: Nanjing Tech University Contract record no.: 2012320000324 Denomination of invention: Decolorizing column and method for performing normal temperature decolorization on DHA grease by employing same Granted publication date: 20111130 License type: Exclusive License Open date: 20101110 Record date: 20120328 |