CN105727592B - A kind of collosol and gel matrix capillary monolithic column and preparation method thereof - Google Patents
A kind of collosol and gel matrix capillary monolithic column and preparation method thereof Download PDFInfo
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- CN105727592B CN105727592B CN201610059614.6A CN201610059614A CN105727592B CN 105727592 B CN105727592 B CN 105727592B CN 201610059614 A CN201610059614 A CN 201610059614A CN 105727592 B CN105727592 B CN 105727592B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/22—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the construction of the column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
- G01N30/6052—Construction of the column body
- G01N30/6073—Construction of the column body in open tubular form
- G01N30/6078—Capillaries
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/80—Aspects related to sorbents specially adapted for preparative, analytical or investigative chromatography
- B01J2220/84—Capillaries
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/80—Aspects related to sorbents specially adapted for preparative, analytical or investigative chromatography
- B01J2220/86—Sorbents applied to inner surfaces of columns or capillaries
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Abstract
The invention discloses a kind of collosol and gel matrix capillary monolithic column and preparation method thereof.The preparation method is, polymer fluid is filled with the capillary 10cm of the alkenyl Microwave Emulsifier-Free Polymerization 14.5min under the conditions of 80 DEG C of temperature, power 700W.The present invention is prepared for collosol and gel capillary monolithic column by temperature control microwave synthesizer in-situ polymerization in capillary.Chromatographic performance evaluation is carried out to prepared integral post under electrochromatography (P CEC) clastotype of pressurizeing, baseline separation four kinds of thiocarbamide, naphthalene, toluene and biphenyl materials, wherein can reach 1.83 μm to the minimum theoretical plate height of naphthalene.Contrasted with the experimental result of conventional microwave method, the theoretical cam curve of naphthalene brings up to 54794/m from 10000/m, drastically increases the splitter effect of compound.Scanning electron microscope the result shows that：The collosol and gel capillary monolithic column prepared with temperature control microwave, integral material is evenly distributed and is tightly combined with capillary tube inner wall in its pipe.
Description
Technical field
The present invention relates to capillary monolithic column technology, and in particular to a kind of collosol and gel matrix capillary monolithic column and its system
Preparation Method.
Background technology
Capillary electric chromatogram (CEC) is a kind of micro column liquid chromatography isolation technics using electroosmotic flow as driving force.It is combined
The high selectivity of high performance liquid chromatography (HPLC) and the high efficiency of Capillary Electrophoresis (CE) are a kind of new differential from skill
Art.It has the characteristics that quick separating and sample, reagent consumption less.The separation analysis of ionic compound is not only applicable to, is also used
Analyzed in the separation of neutral compound.
Capillary column is the core of capillary electric chromatogram separation analysis, and the preparation of capillary column is the pass of capillary electric chromatogram
Key.Capillary electric chromatographic column can be divided into following three kinds according to existing way of the stationary phase in column:Open capillary electric chromatographic column,
Filled capillary pipe electric chromatographic column and entire capillary electric chromatographic column.Open capillary electric chromatographic column compared to it is relatively low, column capacity is smaller
And detection sensitivity is low, so its application is received and is subject to certain restrictions.Filled capillary pipe electric chromatographic column is due to needing plunger, column
Plug poor reliability and the porosity of poor, the unmanageable plunger of repeatability, easily lead to zone broadening, bubble etc. generated at plunger
Problem directly influences column effect and reappearance.Comparatively speaking, capillary vessel electric chromatogram monolithic column is no longer needed at capillary both ends
Burn plug, it is considered to be a kind of preparation method got a good chance of that capillary electric chromatogram further develops in the future.
From the classification of Monolithic Columns, can be classified as organic polymer integral post, inorganic sol-gel integral post and
Organic-inorganic hybrid material integral post.Sol-gel technique refers to the gelation process of colloidal sol, i.e., substantially single in liquid medium
Elementary particle develops into three-dimensional net structure-gel.Sol-gel technique has high-purity, high uniformity and the synthesis temperature low etc.
Advantage, is widely used in materials science field in recent years, and sol-gel technique has been used for the preparation of integral post at present.
Monolithic silica column using alkoxy silane as silicon substrate source, its preparation process include two reaction process：First, alkoxy silane
Hydrolysis, polycondensation form net structure；Second, being chemically modified to the silicone hydroxyl on surface, specific retention property is made it have.
Anal.Chem. magazine 2001 year reports D μ Lay etc. in the 16th 3921-3926 pages of the phase of volume 73 and uses methacryloxypropyl
Trimethyl silane solution triggers in the presence of acidic catalyst, water, toluene and a kind of photoinitiator under 365nm has been made more
Hole monolithic silica column, this silicagel column show reverse-phase chromatography behavior, to the neutral compound of small-molecular-weight, such as PAHs, alkyl
Benzene, alkyl phenyl ketone and steroid are separated, are as a result satisfied with.Electrophoresis magazines 2003 year volume 24
3rd 408-420 pages of phase reported Darin etc. and is prepared for surface through C18The monolithic silica column of modification, and to neutral and powered chemical combination
Thing is separated, and in the case where prepared by the column optimized and flow phase composition and flow conditions, average column effect reaches 160000/m.
It is modified more with two that J.Chromatogr.A magazines 2003 year 209-215 pages of the 1-2 phases of volume 1004 report D μ Lay etc.
The sol-gel integral post of hole photopolymerization realizes separation to the amino acid of five derivatizations in 7min.One of them is with two
Methyl octadecyl chlorosilane (DMOS) is modified, another uses the fluoro- 7- nitros -1,2 of 4- again after DMOS is modified, and 3 phenylpropyl alcohols two are disliked
The silicone hydroxyl theoretical cam curves that piperazine seals remnants have reached more than 58700/m.
The research work of integral post at present has focused largely on Development of Novel Monolithic Columns and extends the application side of integral post
Face, and the research to integral post preparation methodology is relatively fewer.Domestic and international common organic polymer entirety column preparation method is basic
On by the way of uv photopolymerization and thermal polymerization.It is, in principle, that using gamma-rays, X-ray, ultraviolet, infrared, microwave
It is possible that even ultrasonic wave, which is radiated or irradiated the organic polymer in situ that carries out in stainless steel tube or capillary,.
Microwave is heating in one kind, have the characteristics that firing rate soon, homogeneous heating without temperature gradient, without hysteresis effect.
Microwave accelerates key factor to be heated for the selection to polar organic matter to chemical reaction, i.e. the thermal effect of microwave.In addition
Viewpoint thinks that microwave is extremely complex to chemical reaction effect, is on the one hand that reactant molecule absorbs microwave energy, improves
Molecular motion velocities, cause molecular motion disorderly and unsystematic, cause the increase of entropy；In addition effect of the microwave to polar molecule, compels
It is moved according to electromagnetic field effect mode, result in the increase of entropy, thus microwave be to the mechanism of action of chemical reaction cannot
Only described with microwave thermal effect.Traditional external heat side in integral post manufacturing process is substituted using Microwave Emulsifier-Free Polymerization mode
Formula, it is possible to which hundreds times of shortening polymerization reaction time, so as to greatly improve the efficiency of manufacture integral post, makes common chromatography work
Author can prepare desired integral post in a few minutes and be possibly realized.
The content of the invention
In order to solve the deficiencies in the prior art, the present invention provides a kind of collosol and gel matrix capillary monolithic column and its system
Preparation Method.
The technical scheme is that：A kind of preparation method of collosol and gel matrix capillary monolithic column, polymer fluid is filled
Enter the capillary 10cm of the alkenyl Microwave Emulsifier-Free Polymerization 14.5min under the conditions of 80 DEG C of temperature, power 700W.
Further improvement of the present invention includes：
The collocation method of the polymer fluid is, by 1150 μ L methyl allyl acyloxypropyl trimethoxysilanes, 300 μ
L0.12M hydrochloric acid, lucifuge stirring 30 minutes, obtains monomer solution at room temperature；Then, by 800 μ L toluene and 50mg dodecyl sulphurs
Sour sodium is added in 200 μ L monomer solutions, stirs 30 minutes at room temperature, it is molten to obtain toluene-monomer containing dodecyl sodium sulfate
Liquid mixed liquor.
0.1M NaOH, H are used in the alkenyl method of the capillary, (1) successively2O, 0.1M HCl solutions rinse 0.5h, so
Rinsed afterwards with water to pH=7；(2) methanol solution rinses, nitrogen drying；(3) by γ-MAPS and methanol by volume 1:1 it is mixed
Close solution to be injected in capillary with syringe, and the both ends of capillary are sealed with rubber stopper, be placed in 60 DEG C of water-baths and react
12h；(4) capillary after alkenyl is dried up stand-by with nitrogen.
Another object of the present invention is to provide a kind of collosol and gel matrix capillary monolithic column, it is according to any of the above-described
Method described in is made.
Invention further provides it is a kind of for collosol and gel matrix capillary monolithic column prepare polymer fluid, its according to
Following steps are made：By 1150 μ L methyl allyl acyloxypropyl trimethoxysilanes, 300 μ L0.12M hydrochloric acid, at room temperature lucifuge stir
Mix 30 minutes, obtain monomer solution；Then, 800 μ L toluene and 50mg dodecyl sodium sulfates are added to 200 μ L monomer solutions
In, stir 30 minutes at room temperature, obtain the toluene containing dodecyl sodium sulfate-monomer solution mixed liquor
The present invention is prepared for collosol and gel capillary monolithic column by temperature control microwave synthesizer in-situ polymerization in capillary.
Chromatographic performance evaluation is carried out to prepared integral post under electrochromatography (P-CEC) clastotype of pressurizeing, baseline separation sulphur
Four kinds of urea, naphthalene, toluene and biphenyl materials, wherein can reach 1.83 μm to the minimum theoretical plate height of naphthalene.With conventional microwave method
Experimental result contrast, the theoretical cam curve of naphthalene brings up to 54794 from 10000/m, drastically increases the splitter of compound
Effect.Scanning electron microscope the result shows that with temperature control microwave prepare collosol and gel capillary monolithic column be evenly distributed in capillary and with
Capillary tube inner wall is tightly combined；And the hole of conventional microwave is larger, and combined with capillary wall not close.
Using temperature control microwave substitute conventional microwave react synthesizer to prepare capillary monolithic column, can effectively control prepare it is whole
The reaction condition of scapus, so as to greatly improve the efficiency for preparing integral post, makes the reappearance of experiment be guaranteed.In addition microtrabeculae
Service life is greatly enhanced, and prepared integral separation medium is tightly combined with capillary tube inner wall, and it is more to be resistant to buffer solution
Secondary flushing, can be used more than 100 times；And capillary microtrabeculae prepared by common non-temperature control, separating medium are combined with capillary tube inner wall
It is insecure, it is used continuously more than 10 times and stationary phase obscission occurs.Repeat to prepare 3 capillarys using identical experiment condition
Pipe integral post, the collosol and gel integral post that under identical chromatographic conditions prepared by conventional microwave method, the reappearance of its retention time are
29.30%-33.65%, and the reappearance of temperature control microwave method is 5.40%-12.31%, its reappearance is more preferable, is conducive to common
Chromatography worker the collosol and gel integral posts of needs is prepared in the case where condition is controllable.
Brief description of the drawings
Fig. 1 is the contrast chromatogram for the integral post that integral post prepared by temperature control microwave of the present invention is prepared with conventional microwave.
Fig. 2 a are the electron microscopes of temperature control microwave integral post.
Fig. 2 b are the partial enlarged views of Fig. 2 a.
Fig. 3 a are the electron microscopes of conventional microwave integral post.
Fig. 3 b are the partial enlarged views of Fig. 3 a.
Embodiment
Elaborate with reference to specific embodiment to the present invention.
Experimental procedure
Reagent：Methyl allyl acyloxypropyl trimethoxysilane, sodium hydroxide, hydrochloric acid, methanol, toluene, dodecyl sulphur
Sour sodium, trishydroxymethylaminomethane (Tris), acetonitrile, naphthalene, toluene, thiocarbamide, benzene, biphenyl.
Preparation process：
The preparation of 2.1 polymer fluids：By 1150 μ L methyl allyl acyloxypropyl trimethoxysilanes, 300 μ L0.12M hydrochloric acid,
Lucifuge stirs 30 minutes at room temperature, obtains monomer solution.Then, 800 μ L toluene and 50mgSDS (dodecyl sodium sulfate) are added
Enter into 200 μ L monomer solutions, stir 30 minutes at room temperature, obtain the toluene containing SDS-monomer solution mixed liquor.
2.2 pretreatment：(1) 0.1M NaOH, H are used successively2O, 0.1M HCl solution rinse 0.5h, are then rushed with water
It is washed till pH=7；(2) methanol solution rinses, nitrogen drying；(3) by γ-MAPS and methanol mixed solution (γ-MAPS：CH3OH=
1:1, v/v) injected with syringe in capillary, and the both ends of capillary are sealed with rubber stopper, be placed in 60 DEG C of water-baths and react
12h；(4) capillary after alkenyl is dried up stand-by with nitrogen.
The preparation of 2.3 collosol and gel integral posts：Polymer fluid is filled with the capillary 10cm after pretreatment, in microwave catalysis
(arrange parameter in synthesizer：Temperature：80 DEG C, power：700W, polymerization time：14.5min) it is polymerize.
Experimental result
As shown in Figure 1, the contrast of temperature control microwave of the present invention and conventional microwave：a:Temperature control microwave (polymerization length：10cm, gathers
Close temperature：80 DEG C, polymerization time：14.5min)；b：Conventional microwave (polymerization length：10cm, polymerization temperature：Not temperature control, during polymerization
Between：14.5min).
Experiment condition：Pressurization electrochromatography (P-CEC) clastotype：Inlet 10bar+25kV, capillary：Overall length=
35cm；Overall column length=10cm；Effective length (from capillary inlet to detection window)=26.5cm；100μm I.D.；375μm
O.D. sample introduction：15kV×5s；25 DEG C, buffer solution：ACN:2mmol/L Tris=50:50 (v/v), pH=8.0.
Peak sequence：1st, thiocarbamide, 2, toluene, 3, biphenyl, 4, naphthalene.
From figure 1 it appears that temperature control microwave method prepare collosol and gel integral post its to 4 kinds of compound separating effect ratios
Conventional microwave method it is more preferable, chromatographic peak peak shape is narrow, and separating degree is high.This also illustrates integral material polymerization prepared by temperature control microwave method
Closely, so four kinds of compounds are effectively maintained in capillary column.
Integral post prepared by 1 conventional microwave of table is contrasted with integral post column of the present invention effect
From table 1 it can clearly be seen that integral post separating degree higher of the present invention, four kinds of compounds are obtained for divides well
From.And the column effect of the compound naphthalene of last appearance is 54794/m, is 24 times of conventional microwave method.
From Fig. 2 a, 2b, 3a and 3b electron microscope in as can be seen that integral post of the present invention polymerization well, with capillary wall knot
Close closer, without gap, the electromicroscopic photograph of partial enlargement can be seen that integral material aggregated particles are more delicate, and centre has micro-
Hole and mesoporous can pass through mobile phase.And have larger gap on conventional microwave electromicroscopic photograph, between integral material and capillary, with capillary
Tube wall combination is less close, sees that hole is larger on partial enlarged view.
The present invention is prepared for collosol and gel capillary monolithic column by temperature control microwave synthesizer in-situ polymerization in capillary.
Chromatographic performance evaluation is carried out to prepared integral post under electrochromatography (P-CEC) clastotype of pressurizeing, baseline separation sulphur
Four kinds of urea, naphthalene, toluene and biphenyl materials, wherein can reach 1.83 μm to the minimum theoretical plate height of naphthalene.With conventional microwave method
Experimental result contrast, the theoretical cam curve of naphthalene brings up to 54794/m from 10000/m, drastically increases the separation of compound
Column is imitated.Scanning electron microscope with collosol and gel capillary monolithic column prepared by temperature control microwave in capillary the result shows that be evenly distributed simultaneously
It is tightly combined with capillary tube inner wall；And the hole of conventional microwave is larger, and combined with capillary wall not close.
Using temperature control microwave substitute conventional microwave react synthesizer to prepare capillary monolithic column, can effectively control prepare it is whole
The reaction condition of scapus, so as to greatly improve the efficiency for preparing integral post, makes the reappearance of experiment be guaranteed.In addition microtrabeculae
Service life is greatly enhanced, and prepared integral separation medium is tightly combined with capillary tube inner wall, and it is more to be resistant to buffer solution
Secondary flushing, can be used more than 100 times；And capillary microtrabeculae prepared by common non-temperature control, separating medium are combined with capillary tube inner wall
It is insecure, it is used continuously more than 10 times and stationary phase obscission occurs.Repeat to prepare 3 capillarys using identical experiment condition
Pipe integral post, the collosol and gel integral post that under identical chromatographic conditions prepared by conventional microwave method, the reappearance of its retention time are
29.30%-33.65%, and the reappearance of temperature control microwave method is 5.40%-12.31%, its reappearance is more preferable, is conducive to common
Chromatography worker the collosol and gel integral posts of needs is prepared in the case where condition is controllable.
The basic principles, main features and the advantages of the invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (2)
1. a kind of preparation method of collosol and gel matrix capillary monolithic column, it is characterised in that polymer fluid is filled with alkenyl
Capillary 10cm Microwave Emulsifier-Free Polymerization 14.5min under the conditions of 80 DEG C of temperature, power 700W；The collocation method of the polymer fluid is to incite somebody to action
1150 μ L methyl allyl acyloxypropyl trimethoxysilanes, 300 μ L0.12M hydrochloric acid, lucifuge stirring 30 minutes, obtains list at room temperature
Liquid solution；Then, 800 μ L toluene and 50mg dodecyl sodium sulfates are added in 200 μ L monomer solutions, stir 30 at room temperature
Minute, obtain the toluene containing dodecyl sodium sulfate-monomer solution mixed liquor；The alkenyl method of the capillary,（1）Successively
With 0.1M NaOH, H2O, 0.1M HCl solutions rinse 0.5 h, are then rinsed with water to pH=7；（2）Methanol solution rinses, nitrogen
Air-blowing is done；（3）By γ-MAPS and methanol by volume 1:1 mixed solution is with syringe injection capillary, and by capillary
Both ends sealed with rubber stopper, be placed in 60 DEG C of water-baths and react 12 h；（4）Capillary nitrogen drying after alkenyl is treated
With.
A kind of 2. collosol and gel matrix capillary monolithic column, it is characterised in that it is made in accordance with the method for claim 1, should
Integral post integral material aggregated particles are fine and closely woven, and there are micropore and mesoporous in centre；Aggregated particles combined with capillary wall it is closer, with reference to
Locate no gap.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103071314A (en) * | 2011-10-25 | 2013-05-01 | 天津科技大学 | Preparation method for novel ionic liquid capillary monolithic column |
| CN103433008A (en) * | 2013-09-13 | 2013-12-11 | 河南科技学院 | Hollow-fiber-film-coated molecular imprinting integral adsorption rod, as well as preparation method and application thereof |
| CN103721669A (en) * | 2013-12-10 | 2014-04-16 | 天津大学 | Preparation method of silica gel hybridization capillary tube monolithic column |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103071314A (en) * | 2011-10-25 | 2013-05-01 | 天津科技大学 | Preparation method for novel ionic liquid capillary monolithic column |
| CN103433008A (en) * | 2013-09-13 | 2013-12-11 | 河南科技学院 | Hollow-fiber-film-coated molecular imprinting integral adsorption rod, as well as preparation method and application thereof |
| CN103721669A (en) * | 2013-12-10 | 2014-04-16 | 天津大学 | Preparation method of silica gel hybridization capillary tube monolithic column |
Non-Patent Citations (2)
| Title |
|---|
| 微波聚合快速制备分子印迹毛细管电色谱整体柱;张裕平等;《高等学校化学学报》;20070930;第28卷(第9期);1654-1655 * |
| 毛细管硅胶基质整体柱的制备及其电色谱性能研究;邵华等;《色谱》;20050531;第23卷(第3期);244 * |
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