CN102636602B - Neutral hydrophilically-interacted hybrid silicagel-based monolithic column - Google Patents
Neutral hydrophilically-interacted hybrid silicagel-based monolithic column Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000000741 silica gel Substances 0.000 title claims abstract description 28
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 28
- 230000007935 neutral effect Effects 0.000 title claims abstract description 16
- 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 6
- 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 19
- 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 9
- 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 10
- 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
- 238000005370 electroosmosis Methods 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
- 230000035699 permeability Effects 0.000 abstract 1
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 7
- 239000000377 silicon dioxide Substances 0.000 description 7
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 6
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 4
- ISAKRJDGNUQOIC-UHFFFAOYSA-N Uracil Chemical compound O=C1C=CNC(=O)N1 ISAKRJDGNUQOIC-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
- 238000006116 polymerization reaction Methods 0.000 description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 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
- 230000000694 effects Effects 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
- 238000000034 method Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002777 nucleoside Substances 0.000 description 2
- 125000003835 nucleoside group Chemical group 0.000 description 2
- 239000002718 pyrimidine nucleoside Substances 0.000 description 2
- ZENDWEPAVHORFD-UHFFFAOYSA-N pyrimidine;urea Chemical compound NC(N)=O.C1=CN=CN=C1 ZENDWEPAVHORFD-UHFFFAOYSA-N 0.000 description 2
- 229940035893 uracil Drugs 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
- 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
- 238000001962 electrophoresis Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 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
- 230000008569 process Effects 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
- 238000012360 testing method Methods 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 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 a kind of micro-isolation technics rapidly and efficiently of development in recent years, and capillary electric chromatographic column, as the core of CEC technology application, has become a study hotspot of modern micro-separation field.Capillary monolithic column has that preparation is simple, inner structure is even, surface modification is versatile and flexible, bio-compatibility is good and without advantages such as sintering plungers, in CEC piece-rate system, is widely used.
The integral body of the class new role pattern that neutral integral post is development in recent years is phase fixedly, its feature is that fixedly phase surface produces the group of forceful electric power lotus without dissociating, avoided and charged analyte between produce unnecessary electrostatic interaction, by the electrophoretic migration of charged analyte and the difference of polarity, reach the object to the separation and 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 the group that contains polarity, (Electrophoresis 2005,26,1988 – 1995 still can to produce relatively strong electroosmotic flow; Karenga, S., El Rassi, Z., J. Sep. Sci. 2008,31,2677 – 2685.), thereby be better applied in CEC piece-rate system, realize the compartment analysis fast and efficiently to analyte.At present, the non-charge type integral post of reporting is all the organic polymer integral post of preparing based on organic substrate polyreaction, there is not yet the correlation technique report of neutral integral post prepared by silica matrix material, wherein chief reason is that its surface of silica matrix integral post of preparing by traditional handicraft all contains a large amount of silicon hydroxyls, silicon hydroxyl can produce obvious negative charge effect in wider pH scope, as long as the silica matrix integral post that adopts conventional sol-gel technology to prepare, polymerization Silica Surface will produce silicon hydroxyl, when practical application, need to carry out sealing and process to shield the unnecessary Electrostatic Absorption that silicon hydroxyl produces, this has brought larger difficulty to the non-charge type monolithic silica column of preparation.
Organic inorganic hybridization technology is successfully applied to prepare hybridisation silica gel integral post, cage shape type polyhedron siloxane is the typical organic-inorganic hybrid nanometer material with space multistory conformation that a class is comprised of element silicon and oxygen element, there is good mechanical stability and resistance to acids and bases, and without silicon hydroxyl, contribute 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 one-step polymerization reaction, by cage shape type polyhedron siloxane Application of micron in the neutral hydrophilic interaction hybridisation silica gel integral post of preparation, solved that traditional silicon gel matrix is difficult to eliminate silicon hydroxyl and the problem that is difficult to prepare neutral silica gel integral post, set up non-charge type hydrophilic interaction hybridisation silica gel integral post polyreaction and each component proportion.The prepared monolithic column stationary phase of the present invention is organic inorganic hybridization silica gel, its surface does not have silicon hydroxyl, solved electrostatic interaction between the silicon hydroxyl of charging cpd and negative charge, contain neutral polar group simultaneously, adsorbable mobile phase intermediate ion also provides certain zeta electromotive force, produces relatively forceful electric power seepage flow, and has typical hydrophilic chromatographic performance, can be applied to preferably the separated demand of CEC piece-rate system, particularly centering and electrically charged compound.
For achieving the above object, the present invention adopts following technical scheme:
A kind of hydrophilic interaction hybridisation silica gel monolithic column stationary phase surface neutral of neutrality and the polarity hydroxyl that contains hydrophilic interaction; Described hybridisation silica gel integral post is formed by the organic inorganic hybridization polyreaction of uncharged polarity organic monomer, poly-cage modle siloxane crosslinker, radical initiator and pore-foaming agent.
Described uncharged polarity organic monomer is methacrylate hydroxyl ethyl ester, and poly-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 azoisobutyronitrile.
In its compositing formula, each component accounts for the number percent that integral post always forms quality and is: polarity organic monomer and poly-cage modle siloxane crosslinker total amount account for 30%, and wherein the consumption of poly-cage modle siloxane crosslinker be 5.1% ~ 7.9% of total composition quality; Initiating agent accounts for 1%; Pore-foaming agent accounts for 69%, and wherein toluene consumption accounts for the 10.9%-35.0% of total composition quality.
Remarkable advantage of the present invention is: the hydrophilic interaction hybridisation silica gel integral post of non-charge type neutrality of the present invention is to adopt free radical to cause in-situ polymerization one step to make, to with the cage shape type polyhedron siloxane nano material of silicon hydroxyl, not introduce the non-charge type hybridisation silica gel integral post of preparation, 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 to be formed by uncharged polarity organic monomer (methacrylate hydroxyl ethyl ester) and poly-cage modle siloxane crosslinker (methyl methacrylate base cage shape oligomeric silsesquioxane) copolymerization, fixedly phase surface is without silicon hydroxyl, solved strong electrostatic adsorption between charging cpd and silicon hydroxyl, contain simultaneously and enrich neutral polar group, adsorbable mobile phase intermediate ion is in fixing phase surface, certain zeta electromotive force is provided, produce relatively forceful electric power seepage flow, and there is typical hydrophilic chromatographic performance, can meet the continuous separation requirement to the neutrality of polarity and charging cpd.
Accompanying drawing explanation
Fig. 1 is the prepared integral post post effect of different proportionings change curve.
Post A: poly-cage modle siloxane crosslinker 7.0%, organic monomer: 23%, lauryl alcohol: 35.0%, toluene: 34.0%, initiating agent 1%.
Post B: poly-cage modle siloxane crosslinker 7.0%, organic monomer: 23%, lauryl alcohol: 26.8%, toluene: 42.2%, initiating agent 1%.
Post C: poly-cage modle siloxane crosslinker 7.0%, organic monomer: 23%, lauryl alcohol: 19.0%, toluene: 50.0%, initiating agent 1%.
Post D: poly-cage modle siloxane crosslinker 7.0%, organic monomer: 23%, lauryl alcohol: 10.9%, toluene: 59.1%, initiating agent 1%.
Post E: poly-cage modle siloxane crosslinker 5.1%, organic monomer: 24.9%, lauryl alcohol: 19.0%, toluene: 50.0%, initiating agent 1%.
Post F: poly-cage modle siloxane crosslinker 6.0%, organic monomer: 24.0%, lauryl alcohol: 19.0%, toluene: 50.0%, initiating agent 1%.
Post G: poly-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 amide-type neutral compound.
0. toluene; 1.N, dinethylformamide; 2.N, N-DMAA; 3. acrylamide; 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 '. peak, interface; 1. uracil; 2. urea pyrimidine nucleoside; 3. adenosine; 4. adenine; 5. cytidine; 6. cytimidine; 7. guanine.
Embodiment
By organic monomer: methacrylate hydroxyl ethyl ester, poly-cage modle siloxane crosslinker: methyl methacrylate base cage shape oligomeric silsesquioxane, initiating agent: azoisobutyronitrile, mixes pore-foaming agent: the mass ratio of toluene-lauryl alcohol is respectively by following data preparation:
Post A: poly-cage modle siloxane crosslinker 7.0%, organic monomer: 23%, lauryl alcohol: 35.0%, toluene: 34.0%, initiating agent 1%.
Post B: poly-cage modle siloxane crosslinker 7.0%, organic monomer: 23%, lauryl alcohol: 26.8%, toluene: 42.2%, initiating agent 1%.
Post C: poly-cage modle siloxane crosslinker 7.0%, organic monomer: 23%, lauryl alcohol: 19.0%, toluene: 50.0%, initiating agent 1%.
Post D: poly-cage modle siloxane crosslinker 7.0%, organic monomer: 23%, lauryl alcohol: 10.9%, toluene: 59.1%, initiating agent 1%.
Post E: poly-cage modle siloxane crosslinker 5.1%, organic monomer: 24.9%, lauryl alcohol: 19.0%, toluene: 50.0%, initiating agent 1%.
Post F: poly-cage modle siloxane crosslinker 6.0%, organic monomer: 24.0%, lauryl alcohol: 19.0%, toluene: 50.0%, initiating agent 1%.
Post G: poly-cage modle siloxane crosslinker 7.9%, organic monomer: 22.1%, lauryl alcohol: 19.0%, toluene: 50.0%, initiating agent 1%.
By potpourri sonic oscillation 20min, after logical nitrogen 10min, inject and use respectively in advance the HCl solution of 0.1 ~ 1mol/L and the pretreated kapillary of NaOH solution of 0.1 ~ 1mol/L, by kapillary closed at both ends, be dipped in 60 ℃ of water-baths and react 12h; After having reacted, by pillar first with rinsing with mobile phase after methyl alcohol, with remove may be residual in kapillary reagent; This post balance 15h under low-voltage or pump pressure state can normally be tested or be saved backup.With acetonitrile: phosphoric acid triethylamine salt buffer (5mmol/L, pH 6.5)=90:10 is mobile phase, separation voltage-3 ~-20 kV, take formamide as test substances, carry out capillary electric chromatographic column sign, as shown in Figure 1, under those proportionings, integral post polymerization is complete, and height equivalent to a theoretical plate changes with the ratio variation of pore-foaming agent and organic monomer.
The integral post C of the above preparation of application, with acetonitrile: phosphoric acid triethylamine salt buffer (5mmol/L, pH6.5)=94:6 is mobile phase, separation voltage is born 20 kV, aux. pressure 1.1MPa, flow rate pump is under the condition of 0.1 mL/min, 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. DMF; 2. N,N-DMAA; 3. acrylamide; 4. acetamide; 5. formamide; 6. thiocarbamide.
The integral post C of the above preparation of application, with acetonitrile: phosphoric acid triethylamine salt buffer (2mmol/L, pH 6.5)=90:10 is mobile phase, separation voltage is born 15 kV, aux. pressure 3.5MPa, flow rate pump is under the condition of 0.1 mL/min, the nucleosides of alkalescence obtains effective separated with base polar compound on this non-charge type hydrophilic interaction hybridisation silica gel electric chromatographic column, and peak shape is symmetrical, and without conditions of streaking, eluting peak is followed successively by: 1. uracil; 2. urea pyrimidine nucleoside; 3. adenosine; 4. adenine; 5. cytidine; 6. cytimidine; 7. guanine.
The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (2)
1. a neutral hydrophilic interaction hybridisation silica gel integral post, is characterized in that: described hybridisation silica gel monolithic column stationary phase surface neutral and the polarity hydroxyl that contains hydrophilic interaction;
Described hybridisation silica gel integral post is formed by the organic inorganic hybridization polyreaction of uncharged polarity organic monomer, poly-cage modle siloxane crosslinker, radical initiator and pore-foaming agent;
Described uncharged polarity organic monomer is methacrylate hydroxyl ethyl ester, and poly-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 azoisobutyronitrile.
2. the hydrophilic interaction hybridisation silica gel integral post of neutrality according to claim 1, it is characterized in that: in its compositing formula, each component accounts for the number percent that integral post always forms quality and is: polarity organic monomer and poly-cage modle siloxane crosslinker total amount account for 30%, and wherein the consumption of poly-cage modle siloxane crosslinker be the 5.1%-7.9% of total composition quality; Initiating agent accounts for 1%; Pore-foaming agent accounts for 69%, and wherein to account for the ratio that pore-foaming agent always forms quality be a kind of in 34%, 42.2%, 50% to toluene consumption.
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| CN104458973B (en) * | 2014-12-09 | 2016-06-29 | 福州大学 | A kind of on-line determination method suitable in 6-(10-hydroxy-6-oxo-trans-1-undecenyl)-.beta.-resorcylic acid lactone and metabolite thereof |
| CN104606924B (en) * | 2015-01-27 | 2017-07-04 | 厦门出入境检验检疫局检验检疫技术中心 | A kind of shitosan is bonded organic silica gel hybridization integral post and preparation method thereof |
| CN104587707B (en) * | 2015-01-30 | 2016-09-07 | 福州大学 | A kind of nano combined hybrid inorganic-organic monolithic silica column and preparation method thereof |
| CN105126388B (en) * | 2015-07-12 | 2017-07-18 | 北京化工大学 | A kind of preparation method of monolithic silica column |
| CN106823466B (en) * | 2017-03-13 | 2019-04-02 | 福州大学 | One metal ion species immobilization modified silica-gel integral post and preparation method thereof |
| CN113385156B (en) * | 2021-06-29 | 2023-08-22 | 江苏大学 | Lipid raft@organic-inorganic hybrid monolithic column and preparation method and application thereof |
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