CN101362074B - Use of double-phenyl hybridization silica gel material monolithic column in chromatogram - Google Patents
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Abstract
The invention relates to a chromatographic analysis technology, in particular to the application of bi-phenylene hybrid silica-gel monolithic column of bridge-bond organic-inorganic hybridization periodically meso-pore separation material in a chromatogram. The specified preparation method of bi-phenylene hybrid silica-gel material adopts a sol-gel method of acid-base catalysis. Under the condition of acid catalysis, hydrolysis reaction is carried out to a monomer, and an alkaline catalyst is added to carry out polycondensation reaction. The reaction rates of the hydrolysis reaction and the polycondensation reaction of the monomer are controlled by controlling and changing the pH value of a reaction system in the reaction process and the hydrolysis reaction and the polycondensation reaction of the monomer are effectively completely separated by the two-step catalysis method so as to obtain monolithic or particle material with uniform frame structure, suitable aperture and periodic meso-pores. Therefore, the chromatographic analysis technology meets the demands of separation, improves processing technology of the internal wall of quartz capillary, obtains stable monolithic separation material, is capable of separating acid, neutral and alkai compounds under the model of capillary electrochromatography, and shows that the material has excellent separation efficiency and separative selectivity.
Description
Technical field
The present invention relates to chromatographic technique, be specially a kind of application of double-phenyl hybridization silica gel material monolithic column in chromatogram of mesoporous parting material of bridged bond type hybrid inorganic-organic cycle.
Background technology
Parting material is the important composition parts that comprise the chromatographic technique of liquid chromatogram, capillary electric chromatogram etc., also be the main material of sample treatment technology such as SPE and SPME, the direct impact analysis efficient of the characteristic of parting material, range of application etc.Along with chromatographic technique progress and application request improve, more and more higher requirement has been proposed also parting material in recent years.
Liquid chromatogram at present commonly used and capillary electric chromatogram parting material mainly contain bonded silica gel material, polymer particles material and based on the integral material of silica gel or polymer etc., silica gel material has the surface nature uniqueness, can still also have problems such as the soda acid of use narrow range, surperficial non-specific adsorption by characteristics such as chemical bonding adjustment form surface properties; Polymeric material has advantages such as acid and alkali-resistance wide ranges, bio-compatibility are good, but material can cause deficiencies such as microstructure change influence separation with using solvent swell.The solution main at above-mentioned deficiency comprises: tight bond silica gel, sealing technology and composite etc. reduce site, non-specific adsorption center, silica gel surface, improve material tolerance acid-base scope, and the modes such as the degree of cross linking that increase polymeric material avoid material microstructure to change with solvent variation.
Though above-mentioned technology improved to a certain extent material physicochemical characteristics, improved separating property, enlarged range of application, avoided deficiency as parting material, but, because the physicochemical characteristics of material own makes so, its shortcoming and defect is still inevitable to a certain extent.New separation material and Study on Preparation Technology are that at present domestic and international association area is mainly studied hot issue, how to obtain having the new material of good separation performance, and the limitation of avoiding traditional parting material performance is common target and pursuit.Inagaki (S.Inagaki, S.Guan, Y.Fukushima, T.Ohsuna, O.Terasaki, Novel Mesoporous Materials with a Uniform Distribution of OrganicGroups and Inorganic Oxide in Their Frameworks, J.Am.Chem.Soc.1999,121,9611-9614.), Stein (B.J.Melde, B.T.Holland, C.F.Blanford, A.Stein, Mesoporous sieves with unified hybrid inorganic/organic frameworks, Chem.Mater.1999,11,3302-3308.) and Ozin (T.Asefa, M.J.Maclachlan, N.Coombs, G.A.Ozin, Periodic mesoporous organosilicas with organic groupsinside the channel walls, Nature 1999,402,867-871.) group has reported in succession that in 1999 bridged bond type hybrid inorganic-organic cycle mesoporous material is called for short the synthetic of PMOs (periodic mesoporousorganosilicas).In the organic-inorganic hybrid mesoporous material of bridged bond type, organo-functional group is uniformly distributed in the skeleton, can not block the duct, occupy pore volume, and flexible organic group can improve the mechanical strength of material, surface parent/hydrophobicity can be regulated by using different organic groups, organic group can also continue to participate in reacting the activated centre of deriving and making new advances, and there are some researches show that this material has better hydrothermal stability and mechanical stability.(C.F.Nie such as Nie, R.Zhao, J.S.Suo, Synthesis and characterization of bifunctional periodic silica with surface andframework benzene functionality, J.Porous Mater.2004,11,141-146.) with cetyl bromination pyrimidine as template, tetraethoxysilane, phenyl triethoxysilane and 1, the two silica-based benzene of the triethoxy cocondensation under acid condition of 4-, prepare novel organic-inorganic hybrid MCM-41 type mesoporous molecular sieve, contained the bridging phenyl of porose inwall and the terminal phenyl in the duct in the material simultaneously.Also there are some documents to introduce the mode (A.Fidalgo of such material structure control, M.E.Rosa, L.M.Ilharco, Chemical control of highly porous silica xerogels:physical propertiesand morphology, Chem.Mater.2003,15,2186-2192.) (D.A.Loy, K.J.Shea, Bridged polysilsesquioxanes.Highly porous hybrid organic-inorganic materials, Chem.Rev.1995,95,1431-1442. (M.P.Kapoor, Q.H.Yang, S.Inagaki, Organizationof phenylene-bridgedhybrid mesoporous silisesquioxane with a crystal-like porewall from a precursor with nonlinear symmetry, Chem.Mater.2004,16,1209-1213.).
Above-mentioned organic and inorganic material combines the characteristics of polymeric material and silica gel material, has good physical characteristic and chemical characteristic, has good prospect as parting material.The particular design of bridging parting material, make material have the stability of polymer and the characteristics of silica gel material special surface character simultaneously, have good stable and stalling characteristic, special vestibule structure by multiple functional group skeletons such as alkyl, thiazolinyl, phenyl ring constitute has very special meaning for improving and adjusting stalling characteristic.
Summary of the invention
The object of the present invention is to provide the application of a kind of double-phenyl hybridization silica gel material monolithic column in chromatogram.
For achieving the above object, the technical solution used in the present invention is: the application of a kind of double-phenyl hybridization silica gel material monolithic column in chromatogram.Described chromatogram can be capillary electric chromatogram, liquid chromatogram or SPE preliminary treatment.
The described double-phenyl hybridization silica gel material monolithic column that is applied in the chromatogram, preparation as follows:
1) preparation double-phenyl hybridization silica gel material: the sol-gel process that adopts acid-base catalysis, the silane precursor of 80-150 μ L is joined in 120-220 μ L methyl alcohol, 12-22 μ L hydrochloric acid and the 10-20 μ L aqueous solution, after mixing, eddy current stirs 1-5min, and at room temperature behind the hydrolysis 3-6h, add the 4-7mg lauryl amine and also mix, stand-by, wherein silane precursor is 1 of the phenyl triethoxysilane of 60-100 μ L and 20-50 μ L, the two silica-based benzene of triethoxy of 4-;
2) the two phenyl integral post of preparation: charge in the pretreated capillary obtaining silica gel material in the step 1), airtight, make silica gel material polymerisation 10-20h under the normal temperature in capillary; Wash 3-5h with absolute ethyl alcohol then,, obtain being applicable to the integral post of chromatographic isolation material again at 40-65 ℃ of following dry 48-72h.
The pretreated process of described capillary is: capillary column is washed 30-45min with 0.2-0.3mol/L hydrochloric acid, water successively, HF with volumetric concentration 10-15% soaks 3-5h down at 35-50 ℃ again, use 1.0-2.0mol/L NaOH, water and washed with methanol 30-45min then, 160-210 ℃ of following logical nitrogen dries up in the gas-chromatography stove at last, and is stand-by.
The integral post volume ratio of gained is after the acetonitrile solution of 1: 1 0.1-0.3mol/L ammoniacal liquor soaks 2-4h, again with the flushing mutually of flowing; After near integral post post bed, the polyimide coating that scrapes off 1-2mm with blade is as detection window, and capillary is packed into after the electrophoresis apparatus cartridge, and the capillary unnecessary two ends cuts.
The silane precursor that adopts during described preparation double-phenyl hybridization silica gel material can be 1, the two silica-based benzene of triethoxy, 1 of 4-, the two silica-based benzene of trimethoxy of 4-, the silica-based ethane of two trimethoxy, the silica-based ethane of two triethoxy, the silica-based propane of two trimethoxy, the silica-based propane of two triethoxy, the silica-based ethene of two trimethoxy, the silica-based ethene of two triethoxy, the silica-based propylene of two trimethoxy or the silica-based propylene of two triethoxy.
Reaction principle: the sol-gel process of two-step catalysis, at first under the acid catalysis condition, monomeric hydrolytically reactive is very fast, and polycondensation reaction is slow, make like this after the abundant hydrolysis of silylating reagent to produce enough silicon hydroxyls, add base catalyst then to accelerate the carrying out of polycondensation reaction.Just effectively the hydrolysis of monomer and polycondensation are ended entirely by this two-step catalysis method.Reaction monomers phenyl triethoxysilane (PTES) end contains phenyl group, and polymerization the back phenyl takes place is distributed in the hole usually.And another monomer 1, the two silica-based benzene of triethoxy (BTEB) of 4-are a kind of two silanization coupling agents with rigid structure, and phenyl group links to each other with two triethoxysilicane groups simultaneously in the molecule, and this part phenyl is distributed in the silica gel skeleton after the polymerization.Therefore, behind PTES and BTEB hydrolytic polymerization, form a kind of special difunctionalization hybrid material.In the skeleton with the hole in the organic group that distributes different retention behaviors can be provided, and have different physicochemical properties, and in prepared material, work simultaneously.The mechanical strength of hybrid material can improve in the phenyl functional group of bridging, and these groups also have certain activity, but because factors such as the pi-electron of space resistance and phenyl and polarity, the functional group that distributes than end active little.But, because the existence of hybrid material jackshaft xenyl functional group, physics, chemistry and the hydrophobic-hydrophilic nmature of whole material all had special influence.
When the BTEB monomer was containing concentration in the methanol in water and is low to moderate 0.2mol/L, under acid or base catalysis, still polymerizable formed gel structure.In reaction system, control the polymerization and the crosslinking degree of gel by adding another kind of monomer PTEB, improve the structural property of gel, the capillary monolithic column that obtains having the appropriate bore structure.
Advantage of the present invention:
The present invention adopt difference in functionality group the bridging silane coupler as raw material, prepared the parting material of the special nature of conjugated polymer and silica gel advantage, mesoporous parting material of bridged bond type hybrid inorganic-organic cycle.
2. bridging parting material of the present invention is by changing the kind of two silane reagents, contain organo-functional group of different nature in two function monomers of its reaction monomers, can obtain having the material of the special vestibule structure of different physical chemistry microenvironment characteristics easily, can improve and adjust stalling characteristic, satisfy the different needs that separate.
3. with the material of double-phenyl hybridization silica gel material of the present invention, have good physical and chemical performance and separation characteristic, have high selectivity and separative efficiency, have special meaning as parting material as capillary electric chromatogram, liquid chromatogram and sample treatment.
4. the preparation double-phenyl hybridization silica gel material adopts the sol-gel process of acid-base catalysis, at first under the acid catalysis condition, monomeric hydrolytically reactive is very fast, and polycondensation reaction is slow, make like this after the abundant hydrolysis of silylating reagent to produce enough silicon hydroxyls, add base catalyst then to accelerate the carrying out of polycondensation reaction, by changing the pH value of reaction system in the control course of reaction, the hydrolysis and the polycondensation reaction speed of control monomer, and just effectively the hydrolysis of monomer and polycondensation are ended entirely by this two-step catalysis method, it is even to obtain skeleton structure, the aperture is fit to has mesoporous integral body or microparticle material of cycle, satisfy separation requirement, improved quartz capillary inwall treatment technology, obtain the stable whole parting material.
5. under the capillary electric chromatogram pattern, new separation material is used for the separation of acidic, neutral and basic compounds, and display material has good separative efficiency, good separation selectivity and range of application.
6. the present invention adopts phenyl triethoxysilane (PTES) and 1, the two silica-based benzene of triethoxy (BTEB) of 4-are as reaction monomers, mesoporous parting material of bridged bond type hybrid inorganic-organic cycle, thus novel double-phenyl hybridization silica gel material monolithic column obtained, it is applied in the chromatography.
7. the present invention adopts the hydrofluoric acid etch method that capillary is carried out preliminary treatment, integral post combines comparatively tight with tube wall as can be seen, it increases greatly for the silicon hydroxy density on the tube wall after handling through hydrofluoric acid etch, thereby carries out the purpose that sol-gel process can reach the fixed leg bed.
Description of drawings
Fig. 1 is the structure chart of raw material coupling agent of the present invention.
Fig. 2 amplifies 5000 times Electronic Speculum figure for double-phenyl hybridization silica gel material of the present invention.
Fig. 3 is the graph of pore diameter distribution of double-phenyl hybridization silica gel material of the present invention.
Fig. 4 separates spectrogram (wherein, the experiment condition: the phase that flows, 5mM Tris-HCl (pH 8.0)+70%ACN of 16 kinds of condensed-nuclei aromatics compounds for adopting bridging parting material of the present invention under the capillary electric chromatogram pattern; Voltage, 10kV.Sample: (1) naphthalene; (2) acenaphthene; (3) fluorenes; (4) acenaphthene; (5) phenanthrene; (6) anthracene; (7) fluoranthene; (8) pyrene; (9) benzo [a] anthracene; (10) bend; (11) benzo [b] fluoranthene; (12) benzo [k] fluoranthene; (13) benzo [a] pyrene; (14) hexichol [a, h] anthracene; (15) indenes [1,2,3-cd] pyrene; (16) benzo [g, h, I] pyrene)
Fig. 5 separates spectrogram (wherein, the experiment condition: 5mM Tris-HCl (pH 8.0)+70%ACN of 8 kinds of alkali compounds for adopting bridging parting material of the present invention under the capillary electric chromatogram pattern; Voltage: 10kV.Sample: (1). antifebrin (pK
b13.39); (2). aniline (pK
b9.42); (3). ortho-aminotoluene (pK
b9.52); (4) .3,4-dimethylaniline (pK
b8.83); (5) .1-naphthylamines (pK
b10.08); (6) .N, accelerine (pK
b8.92); (7). diphenylamines (pK
b13.12); (8) .N, N-diethylaniline (pK
b7.43) .)
Fig. 6 separates spectrogram (wherein, the experiment condition: 5mM Tris-HCl (pH 8.0)+50%ACN of 3 kinds of acid compounds for adopting bridging parting material of the present invention under the capillary electric chromatogram pattern; Voltage: 18kV.Solute: 1. metanitrophenol (pKa8.36); 2. p-nitrophenol (pKa 7.15); 3.o-nitrophenol (pKa 7.23) .)
The specific embodiment
In conjunction with Figure of description, the present invention is described in further detail.
1) capillary preliminary treatment
Capillary column with 0.2mol/L hydrochloric acid, water flushing 30min, soaks 3 h with volumetric concentration 10%HF down at 35 ℃ successively again, uses 1.0mol/L NaOH, water and washed with methanol 30min then, at last in the gas-chromatography stove 160 ℃ down logical nitrogen dry up, stand-by.
2) double-phenyl hybridization silica gel material monolithic column, preparation as follows:
1. prepare double-phenyl hybridization silica gel material: the sol-gel process that adopts acid-base catalysis, silane precursor with 110 μ L, join in 220 μ L methyl alcohol, 22 μ L hydrochloric acid and the 20 μ L aqueous solution, after mixing, eddy current stirs 3min, and at room temperature behind the hydrolysis 4h, adds the 4mg lauryl amine and also mix, stand-by wherein silane precursor is 60 μ L phenyl triethoxysilanes (PTES) and 50 μ L 1, the two silica-based benzene of triethoxy (BTEB) (referring to Fig. 1) of 4-;
2. two phenyl integral post of preparation: step is obtained silica gel material in 1. charge in the capillary, two ends capillaceous link to each other with polyfluortetraethylene pipe, make silica gel material in capillary, with normal temperature reaction 10h down; Wash 3h with absolute ethyl alcohol then,, obtain being applicable to the integral post of parting material in the chromatogram again at 40 ℃ of following dry 48h.
The integral post volume ratio of gained is after the acetonitrile solution of 1: 1 0.1M ammoniacal liquor soaks 4h, again with the sample of preparing the to analyze flushing of using mutually of flowing commonly used.After near integral post post bed, the polyimide coating that scrapes off 1-2mm with blade is as detection window, and capillary is packed into after the electrophoresis apparatus cartridge, and the capillary unnecessary two ends cuts.
3 integral materials characterize condition
The capillary monolithic column that intercepting 5mm is long, at its cross-section metal spraying, JSM-6360LV type SEM (Japanese JEOL company) is used to characterize the microstructure of integral post.The integral material of large volume adopts and the specific embodiment 2) in identical method prepare, to react consumption and amplify 10 times reactant liquor injection 100 * 2.0mm i.d. stainless steel liquid phase gc column tube, react under the operating procedure by above-mentioned double-phenyl hybridization silica gel material monolithic column, after reaction is finished, wash 4h with absolute ethyl alcohol, then integral post is gone out gc column tube, the shape that is cut into small pieces spends the night 80 ℃ of following vacuum drying at last.Poresizer 9310 types press mercury aperture tester (U.S. Micromeritics company) to be used to measure the pore-size distribution (referring to Fig. 2) of integral material.Infrared spectrum measurement adopts Spectrum GX type Fourier transformation infrared spectrometer (U.S. Perkin Elmer company) to measure (referring to Fig. 3) with the KBr pressed disc method.
And capillary separated substituted benzene under the electrochromatography pattern, replica test result (referring to table 1), result show that material has good separation reappearance.
Table 1
Difference from Example 1 is:
1) the pretreated process of capillary is: capillary column is washed 45min with 0.3mol/L hydrochloric acid, water successively, HF with volumetric concentration 15% handles 5h down at 50 ℃ again, use 1.0mol/L NaOH, water and washed with methanol 45min then, 210 ℃ of following logical nitrogen dry up in the gas-chromatography stove at last, and are stand-by.
2) double-phenyl hybridization silica gel material monolithic column, preparation as follows:
1. prepare double-phenyl hybridization silica gel material: the sol-gel process that adopts acid-base catalysis, the silane precursor of 120 μ L is joined in 120 μ L methyl alcohol, 12 μ L hydrochloric acid and the 10 μ L aqueous solution, after mixing, eddy current stirs 5min, and at room temperature behind the hydrolysis 6h, add the 7mg lauryl amine and also mix, stand-by, wherein silane precursor is 1 of the phenyl triethoxysilane of 100 μ L and 20 μ L, the two silica-based benzene of triethoxy of 4-;
2. two phenyl integral post of preparation: step is obtained silica gel material in 1. charge in the pretreated capillary, airtight, make silica gel material polymerisation 20h under the normal temperature in capillary; Wash 5h with absolute ethyl alcohol then,, obtain being applicable to the integral post of chromatographic isolation material again at 65 ℃ of following dry 72h.
Difference from Example 1 is:
1) the pretreated process of capillary is: capillary column is washed 40min with 0.2mol/L hydrochloric acid, water successively, HF with volumetric concentration 13% handles 4h down at 46 ℃ again, use 1.5mo1/L NaOH, water and washed with methanol 40min then, 190 ℃ of following logical nitrogen dry up in the gas-chromatography stove at last, and are stand-by.
2) double-phenyl hybridization silica gel material monolithic column, preparation as follows:
1. prepare double-phenyl hybridization silica gel material: the sol-gel process that adopts acid-base catalysis, the silane precursor of 140 μ L is joined in 160 μ L methyl alcohol, 18 μ L hydrochloric acid and the 15 μ L aqueous solution, after mixing, eddy current stirs 2min, and at room temperature behind the hydrolysis 3h, add the 5mg lauryl amine and also mix, stand-by, wherein silane precursor is 1 of the phenyl triethoxysilane of 90 μ L and 50 μ L, the two silica-based benzene of triethoxy of 4-;
2. two phenyl integral post of preparation: step is obtained silica gel material in 1. charge in the pretreated capillary, airtight, make silica gel material polymerisation 15h under the normal temperature in capillary; Wash 4h with absolute ethyl alcohol then,, obtain being applicable to the integral post of chromatographic isolation material again at 50 ℃ of following dry 65h.
Described silane precursor can be by 90 μ L 1, two silica-based benzene of triethoxy of 4-or 100 μ L 1, and the silica-based benzene of the two trimethoxies of 4-is replaced.
Embodiment 5
Described silane precursor can be replaced by two silica-based ethane of trimethoxy of 80 μ L or the silica-based propane of the two triethoxies of 130 μ L.
Described silane precursor can be by two silica-based ethene of trimethoxy of 140 μ L or the two silica-based propylene of triethoxy of 150 μ L.
Application examples 1:
Capillary column length overall 27cm, effective length 20cm.Prepare double-phenyl hybridization silica gel material monolithic column by embodiment 1 step, then 20 ℃ of temperature, detect wavelength 214nm, data acquiring frequency 16Hz, adopt thiocarbamide as electroendosmotic flow marker, before the experiment, (5mMTris-HCl (pH 8.0)+70%ACN) washes 30min to integral post, uses low-voltage balance 30min then on electrophoresis apparatus with the phase that flows earlier.In the actual analysis process, change the phase time that flows, wash 30min mutually with flowing earlier, again with measuring behind the separation voltage balance 30min.
Adopt bridging parting material of the present invention under the capillary electric chromatogram pattern, to separate 16 kinds of condensed-nuclei aromatics compounds, condition determination: experiment condition: the phase that flows, 5mM Tris-HCl (pH 8.0)+70%ACN; Voltage, 10kV (A).Sample: (1) naphthalene; (2) acenaphthene; (3) fluorenes; (4) acenaphthene; (5) phenanthrene; (6) anthracene; (7) fluoranthene; (8) pyrene; (9) benzo [a] anthracene; (10) bend; (11) benzo [b] fluoranthene; (12) benzo [k] fluoranthene; (13) benzo [a] pyrene; (14) hexichol [a, h] anthracene; (15) indenes [1,2,3-cd] pyrene; (16) benzo [g, h, I] pyrene) (referring to Fig. 4).
Under the mobile phase condition of 70%ACN, except luxuriant and rich with fragrance and anthracene, benzo [a] anthracene with bend two pairs of samples and fail over the branch, other samples have all obtained separation preferably.When operating voltage was 10kV, thiocarbamide went out the peak about 4.8min, and 16 required transit times of sample are 28min.
Application examples 2
Separate 8 kinds of alkali compounds, wherein experiment conditions: 5mM Tris-HCl (pH 8.0)+70%ACN; Voltage: 10kV (A) and 25kV (B).Sample: (1). antifebrin (pK
b13.39); (2). aniline (pK
b9.42); (3). ortho-aminotoluene (pK
b9.52); (4) .3,4-dimethylaniline (pK
b8.83); (5) .1-naphthylamines (pK
b10.08); (6) .N, accelerine (pK
b8.92); (7). diphenylamines (pK
b13.12); (8) .N, N-diethylaniline (pK
b7.43) .)
The separation spectrogram of Fig. 5 amino benzenes compounds on two phenyl integral post, flow mutually for containing 5mM Tris-HCl (pH 8.0) buffer solution of 70%ACN, operating voltage is respectively 10kV, and disengaging time is 10.5min, and eight kinds of amino benzenes compounds all can be obtained preferably and separate.
Application examples 3
The spectrogram that separates 3 kinds of acid compounds, wherein, experiment condition: 5mM Tris-HCl (pH8.0)+50%ACN; Voltage: 18kV.Solute: 1. metanitrophenol (pKa8.36); 2. p-nitrophenol (pKa 7.15); 3.o-nitrophenol (pKa 7.23) .) referring to Fig. 6.
Fig. 6 as can be seen, phenol derivatives has obtained fully separating on integral post, peak sequence is metanitrophenol, p-nitrophenol and o-nitrophenol successively.Because the migratory behaviour of nitrophenols sample on integral post controlled by electrophoresis mechanism and reverse-phase chromatography retention mechanism simultaneously, therefore in electrochromatography, show different separation selectivities.
Claims (1)
1. the application of double-phenyl hybridization silica gel material monolithic column in chromatogram is characterized in that: be applied to the double-phenyl hybridization silica gel material monolithic column in the chromatogram, as follows preparation:
1) preparation double-phenyl hybridization silica gel material: the sol-gel process that adopts acid-base catalysis, the silane precursor of 80-150 μ L is joined in 120-220 μ L methyl alcohol, 12-22 μ L hydrochloric acid and the 10-20 μ L aqueous solution, after mixing, eddy current stirs 1-5min, and at room temperature behind the hydrolysis 3-6h, add the 4-7mg lauryl amine and also mix, stand-by, wherein silane precursor is 1 of the phenyl triethoxysilane of 60-100 μ L and 20-50 μ L, the two silica-based benzene of triethoxy of 4-;
2) the two phenyl integral post of preparation: charge in the pretreated capillary obtaining silica gel material in the step 1), airtight, make silica gel material polymerisation 10-20h under the normal temperature in capillary; Wash 3-5h with absolute ethyl alcohol then,, obtain being applicable to the integral post of chromatographic isolation material again at 40-65 ℃ of following dry 48-72h;
The pretreated process of capillary is: capillary column is washed 30-45min with 0.2-0.3mol/L hydrochloric acid, water successively, HF with volumetric concentration 10-15% soaks 3-5h down at 35-50 ℃ again, use 1.0-2.0mol/L NaOH, water and washed with methanol 30-45min then, 160-210 ℃ of following logical nitrogen dries up in the gas-chromatography stove at last, and is stand-by;
The integral post volume ratio of gained is after the acetonitrile solution of 1: 1 0.1-0.3mol/L ammoniacal liquor soaks 2-4h, again with the flushing mutually of flowing; After near integral post post bed, the polyimide coating that scrapes off 1-2mm with blade is as detection window, and capillary is packed into after the electrophoresis apparatus cartridge, and the capillary unnecessary two ends cuts.
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| CN1527053A (en) * | 2003-03-07 | 2004-09-08 | 江苏康缘药业股份有限公司 | Quality control method for rehmannia prepn of six ingredients |
| CN1554945A (en) * | 2003-12-24 | 2004-12-15 | 厦门大学 | Method for preparing octyl group micro column liquid phase chromatograph integrate column |
| EP1596193A1 (en) * | 2004-04-30 | 2005-11-16 | Agilent Technologies, Inc. | Novel stationary phases for use in high-performance liquid chromatography |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1527053A (en) * | 2003-03-07 | 2004-09-08 | 江苏康缘药业股份有限公司 | Quality control method for rehmannia prepn of six ingredients |
| CN1554945A (en) * | 2003-12-24 | 2004-12-15 | 厦门大学 | Method for preparing octyl group micro column liquid phase chromatograph integrate column |
| EP1596193A1 (en) * | 2004-04-30 | 2005-11-16 | Agilent Technologies, Inc. | Novel stationary phases for use in high-performance liquid chromatography |
Non-Patent Citations (2)
| Title |
|---|
| 严丽娟等.有机-无机杂化硅胶基质整体柱的制备及其电色谱性能.色谱23 5.2005,23(5),499-503. |
| 严丽娟等.有机-无机杂化硅胶基质整体柱的制备及其电色谱性能.色谱23 5.2005,23(5),499-503. * |
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