CN105727592A - Integrated sol-gel matrix capillary column and preparation method thereof - Google Patents
Integrated sol-gel matrix capillary column and preparation method thereof Download PDFInfo
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- CN105727592A CN105727592A CN201610059614.6A CN201610059614A CN105727592A CN 105727592 A CN105727592 A CN 105727592A CN 201610059614 A CN201610059614 A CN 201610059614A CN 105727592 A CN105727592 A CN 105727592A
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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 an integrated sol-gel matrix capillary column and a preparation method thereof. The preparation method comprises the steps: filling 10cm polymerized solution into alkenylation capillary, and then microwave-polymerizing for 14.5min at 80 DEG C and 700W. According to the invention, the integrated sol-gel matrix capillary column is in-situ prepared in the capillary through a temperature-controlling microwave synthesizer. The prepared integrated column is subjected to chromatography performance evaluation under a pressurizing electrochromatography (P-CEC) separating mode; the four matters of thiourea, naphthalene, methylbenzene and biphenyl are subjected to baseline separation; the lowest theoretical plate height of naphthalene can reach 1.83 mu m; compared with an experimental result of a common microwave method, the result is that the theoretical plate quantity of naphthalene is increased to 54749/m from 10000/m and the separation column effect of the compound is greatly increased. A scanning electron microscope result shows that the integrated materials in the tube of the integrated sol-gel matrix capillary column prepared through the temperature-controlling microwave method are uniformly distributed and are tightly combined with the inner wall of the capillary.
Description
Technical field
The present invention relates to capillary monolithic column technology, be specifically related to a kind of collosol and gel substrate capillary monolithic column and preparation method thereof.
Background technology
Capillary electric chromatogram (CEC) is a kind of micro column liquid chromatography isolation technics with EOF as driving force.It combines height
The high selectivity of effect liquid phase chromatogram (HPLC) and the high efficiency of capillary electrophoresis (CE), be a kind of novel micro separation technique.Its tool
There are the features such as sharp separation and sample, reagent consumption are few.It is not only applicable to the separation analysis of ionic compound, is also used for neutralization
The separation analysis of compound.
Capillary column is that capillary electric chromatogram separates the core analyzed, and the preparation of capillary column is the key of capillary electric chromatogram.Hair
Tubule electric chromatographic column can be divided into following three kinds according to fixing existing way in post: open capillary electric chromatographic column, fills capillary
Pipe electric chromatographic column and entire capillary electric chromatographic column.Open capillary electric chromatographic column compare relatively low, column capacity is less and it is sensitive to detect
Spend low, so its application receives and is subject to certain restrictions.Filled capillary pipe electric chromatographic column is due to needs plunger, plunger poor reliability
Poor with repeatability, be difficult to control to the porosity of plunger, be easily caused zone broadening, at plunger, generate the direct shadow of problem such as bubble
Ring to post effect and repeatability.Comparatively speaking, capillary vessel electric chromatogram monolithic column is no longer necessary to burn stopper at capillary tube two ends, is recognized
For being a kind of preparation method got a good chance of of capillary electric chromatogram development the most further.
From the classification of Monolithic Columns, organic polymer integral post, inorganic sol-gel integral post and organic nothing can be classified as
Machine hybrid material integral post.Sol-gel technique refers to that the elementary cell particle in the gelation process of colloidal sol, i.e. liquid medium is sent out
Exhibition is three-dimensional net structure-gel.Sol-gel technique has the advantages such as high-purity, high uniformity and synthesis temperature are low, in recent years
Being widely used at material science, current sol-gel technique has been used for the preparation of integral post.With alkoxy silane
For the monolithic silica column in silica-based source, its preparation process includes two courses of reaction: one is alkoxy silane hydrolysis, polycondensation formation
Network structure；Two is that the silicone hydroxyl to surface is chemically modified so that it is have specific retention property.Anal.Chem. magazine
Volume 73 the 16th phase calendar year 2001 3921-3926 page reports the methacryloxypropyl trimethyl silane solution such as D μ Lay
In the presence of acidic catalyst, water, toluene and a kind of light trigger at 365nm under cause and prepared Bio-sil integral post,
This silicagel column shows reversed phase chromatography behavior, the neutral compound to small-molecular-weight, such as PAHs, alkylbenzene, alkyl phenyl ketone
And steroid separates, result is satisfied.Electrophoresis magazine volume 24 the 3rd phase 408-420 in 2003
Page reports Darin etc. and is prepared for surface through C18The monolithic silica column modified, and centering and charging cpd separated,
Under the post preparation optimized and flowing phase composition and flow conditions, average post effect reaches 160000/m.J.Chromatogr.A is miscellaneous
Will 2003 volume 1004 1-2 phase 209-215 page report the colloidal sol of two modified hole opticals polymerizations such as D μ Lay-
Gel integral post achieves separation to the aminoacid of five derivatizations in 7min.One of them uses dimethyl stearyl chlorine silicon
Alkane (DMOS) is modified, and another uses again 4-fluoro-7-nitro-1 after DMOS modifies, and 2,3 phenylpropyl alcohol dioxazines seal the silicon hydroxyl of remnants
Base. theoretical cam curve has reached more than 58700/m.
The research work of integral post has focused largely on Development of Novel Monolithic Columns and the application aspect of extension integral post at present, and right
The research of integral post preparation methodology is relatively fewer.The most conventional organic polymer integral post preparation method the most all uses purple
Outer photopolymerization and the mode of thermal polymerization.It is, in principle, that use gamma-rays, X-ray, ultraviolet, infrared, microwave is the most ultrasonic
Ripple carry out radiating or irradiation to carry out organic polymer in situ in stainless steel tube or capillary tube be possible.
Microwave is heating in one, has that firing rate is fast, homogeneous heating is without thermograde, without features such as hysteresis effects.Microwave
It is the heating of the selection to polar organic matter that chemical reaction accelerates key factor, i.e. the thermal effect of microwave.Other viewpoint is recognized
It is extremely complex for microwave to chemical reaction effect, is on the one hand that reactant molecule absorbs microwave energy, improve molecule fortune
Dynamic speed, causes molecular motion disorderly and unsystematic, causes the increase of entropy；The additionally microwave effect to polar molecule, force its according to
Electromagnetic field effect mode is moved, and result in the increase of entropy, and therefore microwave is can not only to use microwave to the mechanism of action of chemical reaction
Thermal effect describes.Microwave Emulsifier-Free Polymerization mode is used to substitute the traditional external heating mode in integral post manufacturing process, it is possible to number
The shortening polymerization reaction time of Radix Achyranthis Bidentatae, thus it is greatly improved the efficiency manufacturing integral post, make the common chromatograph worker all can be several
Prepare the integral post wanted in minute to be possibly realized.
Summary of the invention
In order to solve the deficiencies in the prior art, the invention provides a kind of collosol and gel substrate capillary monolithic column and preparation method thereof.
The technical scheme is that the preparation method of a kind of collosol and gel substrate capillary monolithic column, polymer fluid is filled with thiazolinyl
The capillary tube 10cm Microwave Emulsifier-Free Polymerization 14.5min under the conditions of temperature 80 DEG C, power 700W changed.
Further improvement of the present invention includes:
The collocation method of described polymer fluid is, by 1150 μ L methyl allyl acyloxypropyl trimethoxysilanes, 300 μ L0.12M salt
Acid, under room temperature, lucifuge stirs 30 minutes, obtains monomer solution；Then, by 800 μ L toluene and 50mg dodecyl sodium sulfates
Join in 200 μ L monomer solutions, stir 30 minutes under room temperature, obtain the toluene-monomer solution containing dodecyl sodium sulfate and mix
Close liquid.
The alkenyl method of described capillary tube, (1) is successively with 0.1M NaOH, H2O, 0.1M HCl solution rinses 0.5h,
Then rinse to pH=7 with water；(2) methanol solution rinses, and nitrogen dries up；(3) by γ-MAPS and methanol 1:1 by volume
Mixed solution inject in capillary tube with syringe, and the two ends of capillary tube rubber stopper is sealed, is placed in 60 DEG C of water-baths reaction
12h；(4) the capillary tube nitrogen after alkenyl dries up stand-by.
Another object of the present invention is to provide a kind of collosol and gel substrate capillary monolithic column, it is according to described in any of the above-described item
Method prepare.
Invention further provides a kind of polymer fluid prepared for collosol and gel substrate capillary monolithic column, it is according to following step
Rapid prepared: by 1150 μ L methyl allyl acyloxypropyl trimethoxysilanes, 300 μ L0.12M hydrochloric acid, lucifuge stirring 30 under room temperature
Minute, obtain monomer solution；Then, 800 μ L toluene and 50mg dodecyl sodium sulfate are joined 200 μ L monomer solutions
In, stir 30 minutes under room temperature, must be containing the toluene-monomer solution mixed liquor of dodecyl sodium sulfate
The present invention is prepared for collosol and gel capillary monolithic column by temperature control microwave synthesizer in-situ polymerization in capillary tube.In pressurization
Under electrochromatography (P-CEC) clastotype, prepared integral post has been carried out chromatographic performance evaluation, baseline separation thiourea, naphthalene,
Toluene and four kinds of materials of biphenyl, wherein can reach 1.83 μm to the minimum theoretical plate height of naphthalene.Experiment with conventional microwave method is tied
Fruit contrast, the theoretical cam curve of naphthalene brings up to 54794 from 10000/m, drastically increases the detached dowel effect of compound.Scanning
Electronic Speculum result shows that the collosol and gel capillary monolithic column prepared with temperature control microwave is evenly distributed and and capillary tube inner wall in capillary tube
It is tightly combined；And the hole of conventional microwave is relatively big, and be combined the tightst with capillary wall.
Use temperature control microwave to substitute conventional microwave and device be synthesized to prepare capillary monolithic column, can effectively control to prepare integral post
Reaction condition, thus it is greatly improved the efficiency of preparation integral post, make the repeatability of experiment be guaranteed.The additionally use longevity of microtrabeculae
Life is greatly enhanced, and prepared integral separation medium is tightly combined with capillary tube inner wall, is resistant to buffer solution and repeatedly rinses,
More than 100 times can be used；And the capillary tube microtrabeculae that commonly prepared by non-temperature control, separating medium is combined insecure with capillary tube inner wall,
Use continuously more than 10 times and fixing phase obscission i.e. occurs.Identical experiment condition is used to repeat to prepare 3 capillary integral post,
The collosol and gel integral post that under identical chromatographic conditions prepared by conventional microwave method, the repeatability of its retention time is
29.30%-33.65%, and the repeatability of temperature control microwave method is 5.40%-12.31%, its repeatability is more preferable, the most common color
Spectrum worker prepares the collosol and gel integral post of needs in the case of condition is controlled.
Accompanying drawing explanation
Fig. 1 is the contrast color spectrogram of the integral post that integral post prepared by temperature control microwave of the present invention is prepared with conventional microwave.
Fig. 2 a is the Electronic Speculum figure of temperature control microwave integral post.
Fig. 2 b is the partial enlarged drawing of Fig. 2 a.
Fig. 3 a is the Electronic Speculum figure of conventional microwave integral post.
Fig. 3 b is the partial enlarged drawing of Fig. 3 a.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is elaborated.
Experimental procedure
Reagent: methyl allyl acyloxypropyl trimethoxysilane, sodium hydroxide, hydrochloric acid, methanol, toluene, dodecyl sodium sulfate,
Trishydroxymethylaminomethane (Tris), acetonitrile, naphthalene, toluene, thiourea, 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, room temperature
Lower lucifuge stirs 30 minutes, obtains monomer solution.Then, by 800 μ L toluene and 50mgSDS (dodecyl sodium sulfate)
Join in 200 μ L monomer solutions, stir 30 minutes under room temperature, must be containing the toluene-monomer solution mixed liquor of SDS.
2.2 pretreatments: use 0.1M NaOH, H the most successively2O, 0.1M HCl solution rinses 0.5h, then rushes with water
It is washed till pH=7；(2) methanol solution rinses, and nitrogen dries up；(3) by γ-MAPS and methanol mixed solution (γ-MAPS:
CH3OH=1:1, v/v) inject in capillary tube with syringe, and the two ends of capillary tube rubber stopper is sealed, it is placed in 60 DEG C
Water-bath is reacted 12h；(4) the capillary tube nitrogen after alkenyl dries up stand-by.
The preparation of 2.3 collosol and gel integral post: polymer fluid is filled with the capillary tube 10cm after pretreatment, at microwave catalysis synthesizer
Interior (arranging parameter: temperature: 80 DEG C, power: 700W, polymerization time: 14.5min) is polymerized.
Experimental result
As it is shown in figure 1, the contrast of temperature control microwave of the present invention and conventional microwave: a: temperature control microwave (it is polymerized length: 10cm, poly-
Conjunction temperature: 80 DEG C, polymerization time: 14.5min)；B: conventional microwave (polymerization length: 10cm, polymerization temperature: not temperature control,
Polymerization time: 14.5min).
Experiment condition: pressurization electrochromatography (P-CEC) clastotype: inlet 10bar+25kV, capillary tube: 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: 1, thiourea, 2, toluene, 3, biphenyl, 4, naphthalene.
From figure 1 it appears that the collosol and gel integral post prepared of temperature control microwave method its to 4 kinds of compound separating effects than common
Microwave method 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 table 1 conventional microwave and integral post post of the present invention effect contrast
From table 1 it can clearly be seen that integral post separating degree of the present invention is higher, four kinds of compounds are obtained for well separation.And
And the post effect of last compound naphthalene going out peak is 54794/m, it it is 24 times of conventional microwave method.
It can be seen that integral post of the present invention polymerization is good from the Electronic Speculum figure of Fig. 2 a, 2b, 3a and 3b, be combined with capillary wall
Relatively tight, there is no space, the electromicroscopic photograph of partial enlargement is it can be seen that integral material aggregated particles is more delicate, and there is micropore centre
Can be by flowing phase with mesopore.And on conventional microwave electromicroscopic photograph, between integral material and capillary tube, have bigger space, with capillary tube
Wall combines less tight, partial enlarged drawing is seen hole is bigger.
The present invention is prepared for collosol and gel capillary monolithic column by temperature control microwave synthesizer in-situ polymerization in capillary tube.In pressurization
Under electrochromatography (P-CEC) clastotype, prepared integral post has been carried out chromatographic performance evaluation, baseline separation thiourea, naphthalene,
Toluene and four kinds of materials of biphenyl, wherein can reach 1.83 μm to the minimum theoretical plate height of naphthalene.Experiment with conventional microwave method is tied
Fruit contrast, the theoretical cam curve of naphthalene brings up to 54794/m from 10000/m, drastically increases the detached dowel effect of compound.Sweep
Retouch Electronic Speculum result show the collosol and gel capillary monolithic column prepared with temperature control microwave be evenly distributed in capillary tube and with in capillary tube
Wall is tightly combined；And the hole of conventional microwave is relatively big, and be combined the tightst with capillary wall.
Use temperature control microwave to substitute conventional microwave and device be synthesized to prepare capillary monolithic column, can effectively control to prepare integral post
Reaction condition, thus it is greatly improved the efficiency of preparation integral post, make the repeatability of experiment be guaranteed.The additionally use longevity of microtrabeculae
Life is greatly enhanced, and prepared integral separation medium is tightly combined with capillary tube inner wall, is resistant to buffer solution and repeatedly rinses,
More than 100 times can be used；And the capillary tube microtrabeculae that commonly prepared by non-temperature control, separating medium is combined insecure with capillary tube inner wall,
Use continuously more than 10 times and fixing phase obscission i.e. occurs.Identical experiment condition is used to repeat to prepare 3 capillary integral post,
The collosol and gel integral post that under identical chromatographic conditions prepared by conventional microwave method, the repeatability of its retention time is
29.30%-33.65%, and the repeatability of temperature control microwave method is 5.40%-12.31%, its repeatability is more preferable, the most common color
Spectrum worker prepares the collosol and gel integral post of needs in the case of condition is controlled.
The ultimate principle of the present invention and principal character and advantages of the present invention have more than been shown and described.The technical staff of the industry should
This understanding, the present invention is not restricted to the described embodiments, and the simply explanation present invention's described in above-described embodiment and description is former
Reason, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, these changes and improvements
Both fall within scope of the claimed invention.Claimed scope is defined by appending claims and equivalent thereof.
Claims (5)
1. the preparation method of a collosol and gel substrate capillary monolithic column, it is characterised in that polymer fluid is filled with the capillary of alkenyl
Pipe 10cm is Microwave Emulsifier-Free Polymerization 14.5min under the conditions of temperature 80 DEG C, power 700W.
The preparation method of a kind of collosol and gel substrate capillary monolithic column the most according to claim 1, it is characterised in that described
The collocation method of polymer fluid is, by 1150 μ L methyl allyl acyloxypropyl trimethoxysilanes, and 300 μ L0.12M hydrochloric acid,
Under room temperature, lucifuge stirs 30 minutes, obtains monomer solution；Then, by 800 μ L toluene and 50mg dodecyl sodium sulfates
Joining in 200 μ L monomer solutions, stir 30 minutes under room temperature, the toluene-monomer that must contain dodecyl sodium sulfate is molten
Liquid mixed liquor.
The preparation method of a kind of collosol and gel substrate capillary monolithic column the most according to claim 1, it is characterised in that described
The alkenyl method of capillary tube, (1) is successively with 0.1M NaOH, H2O, 0.1M HCl solution rinses 0.5h, then
Rinse to pH=7 with water；(2) methanol solution rinses, and nitrogen dries up；(3) by γ-MAPS and methanol 1:1 by volume
Mixed solution inject in capillary tube with syringe, and the two ends of capillary tube rubber stopper is sealed, is placed in 60 DEG C of water-baths
Reaction 12h；(4) the capillary tube nitrogen after alkenyl dries up stand-by.
4. a collosol and gel substrate capillary monolithic column, it is characterised in that prepare according to the method described in any one of claim 1-3.
5. the polymer fluid prepared for collosol and gel substrate capillary monolithic column, it is characterised in that prepare according to following steps:
By 1150 μ L methyl allyl acyloxypropyl trimethoxysilanes, 300 μ L0.12M hydrochloric acid, under room temperature, lucifuge stirs 30 minutes,
Obtain monomer solution；Then, 800 μ L toluene and 50mg dodecyl sodium sulfate are joined in 200 μ L monomer solutions,
Stir 30 minutes under room temperature, must be containing the toluene-monomer solution mixed liquor of dodecyl sodium sulfate.
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| CN111617516A (en) * | 2020-07-10 | 2020-09-04 | 安徽师范大学 | Silica gel integral open-tube capillary column with metal wire as template and preparation method thereof |
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| CN103071314A (en) * | 2011-10-25 | 2013-05-01 | 天津科技大学 | Preparation method for novel ionic liquid capillary monolithic column |
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| 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 |
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