CN102636602A - Neutral hydrophilically-interacted hybrid silicagel-based monolithic column - Google Patents
Neutral hydrophilically-interacted hybrid silicagel-based monolithic column Download PDFInfo
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- CN102636602A CN102636602A CN2012101060918A CN201210106091A CN102636602A CN 102636602 A CN102636602 A CN 102636602A CN 2012101060918 A CN2012101060918 A CN 2012101060918A CN 201210106091 A CN201210106091 A CN 201210106091A CN 102636602 A CN102636602 A CN 102636602A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000000741 silica gel Substances 0.000 title claims abstract description 29
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 29
- 230000007935 neutral effect Effects 0.000 title claims abstract description 17
- 229960001866 silicon dioxide Drugs 0.000 title abstract 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 63
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000178 monomer Substances 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 230000005526 G1 to G0 transition Effects 0.000 claims abstract description 9
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical group COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000003999 initiator Substances 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 3
- 239000004971 Cross linker Substances 0.000 claims description 24
- 238000009396 hybridization Methods 0.000 claims description 23
- 230000000977 initiatory effect Effects 0.000 claims description 20
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 16
- 230000003993 interaction Effects 0.000 claims description 15
- 239000004088 foaming agent Substances 0.000 claims description 8
- 239000004615 ingredient Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 14
- 239000010703 silicon Substances 0.000 abstract description 14
- 238000000926 separation method Methods 0.000 abstract description 9
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 3
- 150000001793 charged compounds Chemical class 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 239000003431 cross linking reagent Substances 0.000 abstract 2
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 abstract 1
- 150000000211 1-dodecanols Chemical class 0.000 abstract 1
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical group N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 abstract 1
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical group CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 abstract 1
- 238000005370 electroosmosis Methods 0.000 abstract 1
- 230000035699 permeability Effects 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 9
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 6
- ISAKRJDGNUQOIC-UHFFFAOYSA-N Uracil Chemical compound O=C1C=CNC(=O)N1 ISAKRJDGNUQOIC-UHFFFAOYSA-N 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 4
- OIRDTQYFTABQOQ-KQYNXXCUSA-N adenosine Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](CO)[C@@H](O)[C@H]1O OIRDTQYFTABQOQ-KQYNXXCUSA-N 0.000 description 4
- 239000012491 analyte Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- UYTPUPDQBNUYGX-UHFFFAOYSA-N guanine Chemical compound O=C1NC(N)=NC2=C1N=CN2 UYTPUPDQBNUYGX-UHFFFAOYSA-N 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 239000002777 nucleoside Substances 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 4
- 229940035893 uracil Drugs 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- UNXNGGMLCSMSLH-UHFFFAOYSA-N dihydrogen phosphate;triethylazanium Chemical compound OP(O)(O)=O.CCN(CC)CC UNXNGGMLCSMSLH-UHFFFAOYSA-N 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- UHDGCWIWMRVCDJ-UHFFFAOYSA-N 1-beta-D-Xylofuranosyl-NH-Cytosine Natural products O=C1N=C(N)C=CN1C1C(O)C(O)C(CO)O1 UHDGCWIWMRVCDJ-UHFFFAOYSA-N 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 2
- 229930024421 Adenine Natural products 0.000 description 2
- GFFGJBXGBJISGV-UHFFFAOYSA-N Adenine Chemical compound NC1=NC=NC2=C1N=CN2 GFFGJBXGBJISGV-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000002126 C01EB10 - Adenosine Substances 0.000 description 2
- UHDGCWIWMRVCDJ-PSQAKQOGSA-N Cytidine Natural products O=C1N=C(N)C=CN1[C@@H]1[C@@H](O)[C@@H](O)[C@H](CO)O1 UHDGCWIWMRVCDJ-PSQAKQOGSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229960000643 adenine Drugs 0.000 description 2
- 229960005305 adenosine Drugs 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- UHDGCWIWMRVCDJ-ZAKLUEHWSA-N cytidine Chemical compound O=C1N=C(N)C=CN1[C@H]1[C@H](O)[C@@H](O)[C@H](CO)O1 UHDGCWIWMRVCDJ-ZAKLUEHWSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000011209 electrochromatography Methods 0.000 description 2
- 230000009881 electrostatic interaction Effects 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 125000003835 nucleoside group Chemical group 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- -1 amides compound Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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Abstract
The invention discloses a neutral hydrophilically-interacted hybrid silicagel-based monolithic column which is composed of an uncharged polar organic monomer, a poly-cage type siloxane crosslinking agent, a porogenic agent and an initiator, wherein the uncharged polar organic monomer is hydroxyethyl methacrylate, the poly-cage type siloxane crosslinking agent is methylmethacrylate-based cage-like oligomeric silsesquioxane, the porogenic agent is a mixture of toluene and lauryl alcohols, and the initiator is azodiisobutyronitrile. The polymeric stationary phase of the silicagel-based monolithic column disclosed by the invention is distributed uniformly, the silicagel-based monolithic column is good in permeability and high in mechanical strength, the surface of the stationary phase has no hydroxyl, and the strong electrostatic adsorption between a charged compound and a silicon hydroxyl is solved; and the silicagel-based monolithic column contains rich neutral polar groups, so that the silicagel-based monolithic column can adsorb mobile-phase neutral ions on the surfaces of the stationary phases and provide a certain zeta potential so as to generate a relatively stronger electroosmotic flow, therefore, the silicagel-based monolithic column has a typical hydrophilically-interacted chromatographic performance, and can meet the requirements for the continuous rapid separation of polar neutral and alkaline compound materials.
Description
Technical field
The invention belongs to the analytical chemistry field, be specifically related to a kind of hydrophilic interaction hybridisation silica gel integral post of neutrality.
Background technology
Capillary electric chromatogram (CEC) is that a kind of differential rapidly and efficiently of development in recent years leaves technology, and capillary electric chromatographic column has become the research focus of modern differential from the field as the core of CEC technical application.Capillary monolithic column has that preparation is simple, inner structure is even, surface modification is versatile and flexible, bio-compatibility is good and need not advantage such as sintering plunger, in the CEC piece-rate system, has obtained application widely.
Neutral integral post is the overall fixed phase of one type of new role pattern of development in recent years; Its characteristics are that the stationary phase surface does not have the group of generation forceful electric power lotus that can dissociate; Avoided and charged analyte between produce unnecessary electrostatic interaction; Through the electrophoretic migration of charged analyte and the difference of polarity, reach purpose to the separation and the detection of analyte, received more and more chromatogram workers' concern.In application, though this non-charge type integral post surface does not have the group that can dissociate, as long as contain the group of polarity, (Electrophoresis 2005,26,1988 – 1995 still can to produce relative stronger EOF; Karenga, S., El Rassi, Z., J. Sep. Sci. 2008,31,2677 – 2685.), thereby better application realizes the compartment analysis fast and efficiently to analyte in the CEC piece-rate system.At present; The non-charge type integral post of being reported all is based on the organic polymer integral post of organic substrate polyreaction preparation; Do not see the correlation technique report of the neutral integral post of silica matrix material preparation as yet; Wherein chief reason is all to contain a large amount of silicon hydroxyls through its surface of silica matrix integral post of traditional handicraft preparation; The silicon hydroxyl can produce tangible negative charge effect in wider pH scope, as long as adopt the silica matrix integral post of conventional sol-gel technology preparation, polymerization silica gel surface will produce the silicon hydroxyl; When practical application, need carry out sealing and handle and shield the unnecessary Electrostatic Absorption that the silicon hydroxyl is produced, this has brought big difficulty for the non-charge type monolithic silica column of preparation.
The organic inorganic hybridization technology successfully is applied to prepare the hybridisation silica gel integral post; Cage shape type polyhedron siloxane is one type of typical organic-inorganic hybrid nanometer material with space multistory conformation of being made up of element silicon and oxygen element; Have favorable mechanical stability and resistance to acids and bases; And do not have the silicon hydroxyl, help to prepare non-charge type hybridisation silica gel integral post.
Summary of the invention
The object of the present invention is to provide a kind of hydrophilic interaction hybridisation silica gel integral post of neutrality.The present invention is based on free radical and cause the one-step polymerization reaction; Cage shape type polyhedron siloxane nano material is applied to prepare neutral hydrophilic interaction hybridisation silica gel integral post; Solved that the traditional silicon gel matrix is difficult to eliminate the silicon hydroxyl and the problem that is difficult to prepare the neutral silica gel integral post, set up non-charge type hydrophilic interaction hybridisation silica gel integral post polyreaction and each set of dispense ratio.The prepared integral post stationary phase of the present invention is an organic inorganic hybridization silica gel, and its surface does not have the silicon hydroxyl, has solved electrostatic interaction between the silicon hydroxyl of charging cpd and negative charge; Contain neutral polar group simultaneously; Adsorbable moving phase intermediate ion also provides certain zeta electromotive force, produces relatively than forceful electric power seepage flow, and has typical hydrophilic chromatographic performance; Can be applied to the CEC piece-rate system preferably, particularly to the demand of separating neutral and electrically charged compound.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
A kind of hydrophilic interaction hybridisation silica gel integral post stationary phase of neutrality surface neutral and contain the polarity hydroxyl of hydrophilic interaction; Said hybridisation silica gel integral post is formed by uncharged polarity organic monomer, the organic inorganic hybridization polyreaction of gathering cage modle siloxane crosslinker, radical initiator and pore-foaming agent.
Described uncharged polarity organic monomer is a methacrylate hydroxyl ethyl ester, and gathering the cage modle siloxane crosslinker is methyl methacrylate base cage shape oligomeric silsesquioxane, and pore-foaming agent is the potpourri of toluene and lauryl alcohol, and initiating agent is an azoisobutyronitrile.
Each ingredients constitute integral post is always formed the number percent of quality and is in its compositing formula: the polarity organic monomer with gather cage modle siloxane crosslinker total amount and account for 30%, the consumption that wherein gathers the cage modle siloxane crosslinker is total 5.1% ~ 7.9% of quality of forming; Initiating agent accounts for 1%; Pore-foaming agent accounts for 69%, and wherein the toluene consumption accounts for the 10.9%-35.0% of total composition quality.
Remarkable advantage of the present invention is: the neutral hydrophilic interaction hybridisation silica gel integral post of non-charge type of the present invention is to adopt one step of free radical initiation in-situ polymerization to make; With not introducing the non-charge type hybridisation silica gel integral post of preparation with the cage shape type polyhedron siloxane nano material of silicon hydroxyl; Its inner structure is even; Transparent performance is good, physical strength is high, has solved the problem that traditional handicraft is difficult to prepare non-charge type monolithic silica column.This hydridization type monolithic silica column is by uncharged polarity organic monomer (methacrylate hydroxyl ethyl ester) and gathers cage modle siloxane crosslinker (methyl methacrylate base cage shape oligomeric silsesquioxane) copolymerization and form; The stationary phase surface does not have the silicon hydroxyl; Solved strong electrostatic adsorption between charging cpd and the silicon hydroxyl, contained abundant neutral polar group simultaneously, adsorbable moving phase intermediate ion is in the stationary phase surface; Certain zeta electromotive force is provided; Produce relatively than forceful electric power seepage flow, and have typical hydrophilic chromatographic performance, can satisfy the neutrality of polarity and the continuous separation requirement of charging cpd.
Description of drawings
Fig. 1 is that the prepared integral post post of different proportionings is imitated change curve.
Post A: gather cage modle siloxane crosslinker 7.0%, organic monomer: 23%, lauryl alcohol: 35.0%, toluene: 34.0%, initiating agent 1%.
Post B: gather cage modle siloxane crosslinker 7.0%, organic monomer: 23%, lauryl alcohol: 26.8%, toluene: 42.2%, initiating agent 1%.
Post C: gather cage modle siloxane crosslinker 7.0%, organic monomer: 23%, lauryl alcohol: 19.0%, toluene: 50.0%, initiating agent 1%.
Post D: gather cage modle siloxane crosslinker 7.0%, organic monomer: 23%, lauryl alcohol: 10.9%, toluene: 59.1%, initiating agent 1%.
Post E: gather cage modle siloxane crosslinker 5.1%, organic monomer: 24.9%, lauryl alcohol: 19.0%, toluene: 50.0%, initiating agent 1%.
Post F: gather cage modle siloxane crosslinker 6.0%, organic monomer: 24.0%, lauryl alcohol: 19.0%, toluene: 50.0%, initiating agent 1%.
Post G: gather cage modle siloxane crosslinker 7.9%, organic monomer: 22.1%, lauryl alcohol: 19.0%, toluene: 50.0%, initiating agent 1%.
Fig. 2 is the electrochromatography separation graph of hydrophilic interaction hybridisation silica gel integral post to the amide-type neutral compound.
0. toluene; 1.N, dinethylformamide; 2.N, the N-DMAA; 3. acrylic amide; 4. acetamide; 5. formamide; 6. thiocarbamide.
Fig. 3 is the electrochromatography separation graph of hydrophilic interaction hybridisation silica gel integral post to nucleosides and base alkaline matter.
0. toluene; 0 '. the peak, interface; 1. uracil; 2. uracil nucleosides; 3. adenosine; 4. adenine; 5. cytidine; 6. cytimidine; 7. guanine.
Embodiment
With organic monomer: methacrylate hydroxyl ethyl ester, gather the cage modle siloxane crosslinker: methyl methacrylate base cage shape oligomeric silsesquioxane, initiating agent: azoisobutyronitrile, mix pore-foaming agent: the mass ratio of toluene-lauryl alcohol is respectively by following data preparation:
Post A: gather cage modle siloxane crosslinker 7.0%, organic monomer: 23%, lauryl alcohol: 35.0%, toluene: 34.0%, initiating agent 1%.
Post B: gather cage modle siloxane crosslinker 7.0%, organic monomer: 23%, lauryl alcohol: 26.8%, toluene: 42.2%, initiating agent 1%.
Post C: gather cage modle siloxane crosslinker 7.0%, organic monomer: 23%, lauryl alcohol: 19.0%, toluene: 50.0%, initiating agent 1%.
Post D: gather cage modle siloxane crosslinker 7.0%, organic monomer: 23%, lauryl alcohol: 10.9%, toluene: 59.1%, initiating agent 1%.
Post E: gather cage modle siloxane crosslinker 5.1%, organic monomer: 24.9%, lauryl alcohol: 19.0%, toluene: 50.0%, initiating agent 1%.
Post F: gather cage modle siloxane crosslinker 6.0%, organic monomer: 24.0%, lauryl alcohol: 19.0%, toluene: 50.0%, initiating agent 1%.
Post G: gather cage modle siloxane crosslinker 7.9%, organic monomer: 22.1%, lauryl alcohol: 19.0%, toluene: 50.0%, initiating agent 1%.
With potpourri sonic oscillation 20min, inject behind the logical nitrogen 10min and use the HCl solution of 0.1 ~ 1mol/L and the pretreated kapillary of NaOH solution of 0.1 ~ 1mol/L in advance respectively, with the kapillary closed at both ends, be dipped in 60 ℃ of water-baths and react 12h; After reaction is accomplished, with pillar earlier with behind the methyl alcohol with the moving phase flushing, with remove maybe be residual in the kapillary reagent; Balance 15h under low-voltage or pump pressure state can normally test or preserve subsequent use with this post.With acetonitrile: phosphoric acid triethylamine salt buffer (5mmol/L, pH 6.5)=90:10 is a moving phase, separation voltage-3 ~-20 kV; With the formamide is test substances; Carry out capillary electric chromatographic column and characterize, as shown in Figure 1, under those proportionings; The integral post polymerization is complete, and height equivalent to a theoretical plate changes with the ratio variation of pore-foaming agent and organic monomer.
Use the integral post C of above preparation; With acetonitrile: phosphoric acid triethylamine salt buffer (5mmol/L; PH6.5)=and 94:6 is a moving phase, and it is under the condition of 0.1 mL/min that separation voltage is born 20 kV, aux. pressure 1.1MPa, flow rate pump, and neutral amides compound reaches baseline separation on this non-charge type hydrophilic interaction hybridisation silica gel electric chromatographic column; Eluting peak is followed successively by: 1. N, dinethylformamide; 2. N, the N-DMAA; 3. acrylic amide; 4. acetamide; 5. formamide; 6. thiocarbamide.
Use the integral post C of above preparation; With acetonitrile: phosphoric acid triethylamine salt buffer (2mmol/L, pH 6.5)=90:10 is a moving phase, and it is under the condition of 0.1 mL/min that separation voltage is born 15 kV, aux. pressure 3.5MPa, flow rate pump; The nucleosides of alkalescence is effectively separated on this non-charge type hydrophilic interaction hybridisation silica gel electric chromatographic column with the base polar compound; And peak shape symmetry, no conditions of streaking, eluting peak is followed successively by: 1. uracil; 2. uracil nucleosides; 3. adenosine; 4. adenine; 5. cytidine; 6. cytimidine; 7. guanine.
The above is merely preferred embodiment of the present invention, and all equalizations of doing according to claim of the present invention change and modify, and all should belong to covering scope of the present invention.
Claims (2)
1. the hydrophilic interaction hybridisation silica gel integral post of a neutrality is characterized in that: said hybridisation silica gel integral post stationary phase surface neutral and contain the polarity hydroxyl of hydrophilic interaction;
Said hybridisation silica gel integral post is formed by uncharged polarity organic monomer, the organic inorganic hybridization polyreaction of gathering cage modle siloxane crosslinker, radical initiator and pore-foaming agent;
Described uncharged polarity organic monomer is a methacrylate hydroxyl ethyl ester, and gathering the cage modle siloxane crosslinker is methyl methacrylate base cage shape oligomeric silsesquioxane, and pore-foaming agent is the potpourri of toluene and lauryl alcohol, and initiating agent is an azoisobutyronitrile.
2. the hydrophilic interaction hybridisation silica gel integral post of neutrality according to claim 1; It is characterized in that: each ingredients constitute integral post is always formed the number percent of quality and is in its compositing formula: the polarity organic monomer with gather cage modle siloxane crosslinker total amount and account for 30%, the consumption that wherein gathers the cage modle siloxane crosslinker is total 5.1% ~ 7.9% of quality of forming; Initiating agent accounts for 1%; Pore-foaming agent accounts for 69%, and wherein the toluene consumption accounts for the 10.9%-35.0% of total composition quality.
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| CN104109222A (en) * | 2013-04-22 | 2014-10-22 | 中国科学院大连化学物理研究所 | Preparation of hybrid integral materials containing polyhedral oligomeric silsesquioxane reagent |
| CN104458973A (en) * | 2014-12-09 | 2015-03-25 | 福州大学 | Online determination method suitable for zearalenone and metabolites of zearalenone |
| CN104587707A (en) * | 2015-01-30 | 2015-05-06 | 福州大学 | Nanometer composite organic-inorganic hybrid silica gel monolithic column and preparation method thereof |
| CN104606924A (en) * | 2015-01-27 | 2015-05-13 | 厦门出入境检验检疫局检验检疫技术中心 | Chitosan bonded organic-silica gel hybridization monolithic column and preparation method thereof |
| CN105126388A (en) * | 2015-07-12 | 2015-12-09 | 北京化工大学 | Preparation method of silica gel monolithic column |
| CN106823466A (en) * | 2017-03-13 | 2017-06-13 | 福州大学 | One metal ion species immobilization modified silica-gel integral post and preparation method thereof |
| CN113385156A (en) * | 2021-06-29 | 2021-09-14 | 江苏大学 | Lipid raft @ organic-inorganic hybrid monolithic column and preparation method and application thereof |
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