CN103267825A - Thin-layer chromatoplate having ordered micro-nano structure and manufacturing method thereof - Google Patents
Thin-layer chromatoplate having ordered micro-nano structure and manufacturing method thereof Download PDFInfo
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Abstract
The invention discloses a thin-layer chromatoplate having an ordered micro-nano structure and a manufacturing method thereof. The thin-layer chromatoplate comprises a base plate and a stationary phase on the base plate. The stationary phase comprises a skeleton having an ordered micro-nano inverse opal structure, and a mesoporous microstructure. The skeleton having the ordered micro-nano inverse opal structure is prepared by a photonic crystal film as a template. The surface of the skeleton having the ordered micro-nano inverse opal structure is modified by the mesoporous microstructure. The thin-layer chromatoplate utilizes the photonic crystal having the inverse opal structure as the skeleton. The inverse opal structure can provide enough micro- and nano-mesopores so that a flowing rate can be greatly improved; and a thin-layer chromatographic resolution ratio is obviously improved and good reappearance is obtained. Through combination of the thin-layer chromatogram and photonic crystals, an application scope is greatly expanded.
Description
Technical field
What the present invention relates to is a kind of chromatographic sheet with orderly micro-nano structure and preparation method thereof.It can be used for carrying out the qualitative and semiqualitative analysis of potpourris such as naturalization compound, medicine, chemistry and microorganism composite, is widely used in fields such as quick quality testing, rare metal separation, clinical medicine detection, pesticide residues analysis.
Background technology
Along with improving day by day of industry standard and increasing gradually of practical application, chromatogram has become a flag of 21 century analytical applications uniqueness, and wherein topmost achievement is exactly the discovery of thin-layer chromatography (TLC).A kind of as parallel chromatogram, TLC occupies one seat with advantage such as simple to operate, with low cost in places such as each scientific experiment chamber, factory and schools.
Typical TLC chromatographic process is mainly as follows: the place, an end end and the drying that a spot of determinand are positioned over the fixedly phase of being made up of the adsorbent thin layer, to fix the edge that is added with sample mutually subsequently and immerse by in flowing mutually, flow communication is often formed by two to four kinds of solvent.If it is fixing appropriate with the selection mutually of flowing mutually, because analyte and fixing phase, the phase suction-operated of flowing are different, different component in the potpourri can move fixing mutually with different speed flowing of fixing phase along with flowing, and this process is called as the expansion of chromatogram.After flowability moves to a suitable distance, take out and the fixing phase of rapid draing, by some developers or will fix and place ultraviolet irradiation mutually, can carry out qualitative analysis to the zone that separation obtains.
Characteristics such as thin-layer chromatography is with low cost owing to having, use is simple have the space of developing on a large scale very much at the biochemical analysis detection range.But because silica gel etc. is fixedly due to the constituent lack of alignment of phase, TLC is limited in relatively short length (3-10cm), resolution, experimental result lacks repeatability, and the existence of bonding agent simultaneously also can cause and the secondary interaction of mobile phase and the decline of separation efficiency.Although there has been the row of improvement thin-layer chromatography to improve resolution (as No. 6395178 U.S. Patent application) at present, or other nanostructured thin-layer chromatographys (as No. 20108002930.5 Chinese patent application), but the thin-layer chromatography fixedly introducing of phase lack of alignment and bonding agent or complicated preparation technology makes it be difficult to carry out surperficial little processing to handle again, thereby strengthened the barrier with other detection technique couplings.Its relatively poor reproducibility has seriously limited the application of thin-layer chromatography qualitative and quantitative in fast detecting in addition.Can form the photonic crystal of the micro-nano structure with high-sequential by self assembly, this body structure surface is easy to modify and need not specific apparatus, therefore has application widely at aspects such as biomedicine, materials.When thin-layer chromatography combines with photonic crystal, range of application will be expanded greatly, simultaneously, counter opal structure can provide the mesoporous and mesopore of enough microns and Nano grade, thereby improve flow velocity greatly, the resolution of thin-layer chromatography also has one and promotes and realize respond well reappearance significantly, thereby provides good basis for qualitative detection repeatably.
Up to now, having periodic arrangement is modified with mesoporous counter opal structure film simultaneously and is used for thin-layer chromatography and does not see bibliographical information as yet.
Summary of the invention
Technical matters to be solved by this invention is at above-mentioned the deficiencies in the prior art, have chromatographic sheet and the method for making of orderly micro-nano structure and provide a kind of with lower cost preparation, thereby improve resolution and fidelity factor, lay the foundation for the express-analysis based on thin-layer chromatography detects simultaneously.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of chromatographic sheet with orderly micro-nano structure, comprise substrate and be arranged on fixedly phase on the described substrate, it is characterized in that: described fixing is made up of skeleton and the mesoporous microstructure of the counter opal structure with orderly micro-nano structure mutually, wherein the skeleton of counter opal structure is the template preparation with the photon crystal film, is modified with described mesoporous microstructure on the skeleton surface of counter opal structure.
The macropore diameter of counter opal structure is 200～1000nm, and photon band gap is distributed in the zone of 400～2000nm, and the aperture of mesoporous microstructure is 3～10nm.
Photon crystal film thickness is at 10～120um.
Micro-nano structure is formed by single finely disseminated nano-colloid particle self assembly in order.
Described colloidal particle material is silicon dioxide or polystyrene, and the colloidal particle particle diameter is between 200nm～1um; The material of substrate is silicon dioxide, aluminium oxide, low bulk high temperature borosilicate glass, steel or silicon wafer.
Described single good dispersion nano-colloid particle is that inorganic nano-particle is or/and organic nano particle and their derivant, described inorganic nano-particle comprises non magnetic inorganic nano-particle and magnetic inorganic nano-particle, described non magnetic inorganic nano-particle comprises nonmagnetic metal nano particle and non magnetic nonmetal nano particle, and described derivant comprises and is combined with surface group or/and be coated with the derivant of machine thing.
Described nonmagnetic metal nano particle comprises the oxide nano-particles of silicon oxide particle, Titanium particles or aluminium oxide particles.
Described metal nanoparticle is included as gold particle, gold particle, silver particles, iron particle, palladium particle, chromium particle, nickel particles.
A kind of method of making chromatographic sheet is characterized in that step is as follows:
The first step, with silicon dioxide, pipe/polyhenylethylene nano colloidal particle by gravity deposition, vertical czochralski method or directly coat at substrate and form described orderly micro-nano structure, at least part of photon crystal film with orderly micro-nano structure that forms by self assembly;
Second goes on foot, silicon dioxide, pipe/polyhenylethylene nano colloidal particle is filled and entered in the space of the photon crystal film that assembles by immersion, dropping method;
The 3rd step, with the photon crystal film that assembles as template, remove template by chemical corrosion or high-temperature calcination method, obtain the counter opal structure of periodic arrangement;
The 4th the step, on the surface of counter opal structure utilize graft polymer or depositing silicon gluing method in the photon crystal film finishing mesoporous microstructure of counter opal structure at last, and carry out Development of Thin-Layer Chromatography with this mutually as chromatographic stationary.
Compared with prior art, the present invention has following advantage:
1, chromatographic sheet of the present invention, with the photonic crystal of counter opal structure as skeleton, counter opal structure can provide the mesoporous and mesopore of enough microns and Nano grade, thereby improve flow velocity greatly, the resolution of thin-layer chromatography also has one and promotes and realize respond well reappearance significantly, thin-layer chromatography combines with photonic crystal, and range of application is expanded greatly.
2, the orderly micro-nano structure film of chromatographic sheet of the present invention has certain separating effect, and compares with the commercialization silica gel plate, and required development distance is shorter, can reach lower detectability, and this has important meaning for further raising chromatography resolution.
Description of drawings
Fig. 1 is the schematic top plan view of a kind of embodiment of TLC plate structure.
Dark part is represented to form structure behind the nano-particles filled counter opal space in fact, and dotted portion is represented the meso-hole structure modified.
Embodiment
Below in conjunction with accompanying drawing, the present invention is elaborated:
Embodiments of the present invention relate to TLC plate and relevant manufacture method and use.TLC plate disclosed in this invention can provide the fixedly phase structure of the micro-nano structure of the high-sequential that is suitable for the chromatography purposes, can improve separation efficiency, is beneficial to simultaneously to carry out for modifying mutually with the fixing of other detection technique couplings.
In various embodiments, the TLC plate can be made in the following way: form the micro-nano structure that multilayer order is arranged on fixing phase substrate surface, and be that template makes anti-protein structure with this micro-nano structure, further modify meso-hole structure on its surface subsequently, its structure as shown in Figure 1, dark part is represented to form structure behind the nano-particles filled counter opal space, and dotted portion is represented the meso-hole structure modified.
Fixedly phase substrate is that the structure of TLC plate provides support.The example of baseplate material can comprise, but be not limited to, silicon dioxide, aluminium oxide, low bulk high temperature borosilicate glass are (for example, Pyrex7740 and/or Schott Borofloat glass), steel (for example, stainless steel), silicon wafer or any other high temp glass or other materials that is fit to.In case of necessity, can show substrate and carry out hydrophilic treatment to obtain the condition that better is coated with.
Fixedly phase can put on the corresponding substrate.In one embodiment, the polystyrene colloid particle that single finely disseminated particle diameter is about 1um is scattered in the alcohol, utilize coating machine that colloidal solution is tiled in fixedly on the phase substrate uniformly, colloidal particle is treated can obtain the fixedly phase that surfacing has good micro-nano structure simultaneously after the alcohol volatilization along with the spontaneous arrangement of the volatilization of alcohol forms close-packed structure.Drip and film surface through 80 ℃ of tetraethyl silicate resin precursor solutions (tetraethyl silicate resin, dense HCl, absolute ethyl alcohol equal-volume mix) that are sintered to fix after the structure configured in advance, make in its gap of fully immersing photon crystal film.After behind the drying at room temperature 2h film being placed 500 ℃ of high-temperature calcinations, can obtain to have the silicon dioxide photon crystal film of counter opal structure, further deposit silica gel on the antistructure surface at last, obtain to be modified with the antistructure film of meso-hole structure and to carry out Development of Thin-Layer Chromatography with this mutually as chromatographic stationary.
Be described further below in conjunction with specific embodiment:
Embodiment one
Adopt the St ber method of improvement, prepare the single dispersion solid polystyrene microsphere of particle diameter from tens nanometers to several microns.Draw 1ml, the particle diameter of 2.5vol% is that the PS colloidal solution of 240nm adds in the 20ml ultrapure water, aggressiveness solution before the TEOS that wherein adds 0.3ml subsequently, and it is stand-by to stir 1h under the room temperature.To cross microslide with the Piranha solution-treated vertically inserts in the precursor solution that configures, put into the constant temperature oven drying after leaving standstill 2d under 65 ℃, baking temperature is controlled at 105-110 ℃, about 2-3 hour drying time, after the oven dry, be cooled to room temperature after it is inserted in the muffle furnace 500 ℃ of calcining 4h.Utilize SEM observation, the TLC film that obtains as can be known has counter opal structure.At last, the counter opal structure that makes is immersed 24h in the silica gel solution that utilizes block copolymer surfactant prehydrolysis, make mesoporous silica gel be deposited on the inverse opal structural membrane surface.
By the separation that mixes fluorescein being assessed the thin-layer chromatography effect of prepared film.Mix fluorescein and formed by uranin and rhodamine B, be diluted to 10 with ethanol before the point sample
-2M, 10
-3M and 10
-4M also mixes.Launching used film is that the polystyrene microsphere of 0.9g/ml, particle diameter 1um is coated microslide and formed through sol-gel method and calcining back by concentration, and thickness is about 28um.Utilize the blunt mouthful of glass capillary absorption～10nl potpourri of internal diameter 43um to carry out parallel point sample, point of sample interval～4mm is positioned at upper edge, film bottom～3mm place.
Chromatographic resolution is carried out in small-sized vertical expansion cylinder and homemade parallel TLC development chamber.Before launching with the toluene of 3:7 volume ratio and normal hexane is added into liquid-accumulating chamber as developping agent and conditioning chamber carries out presaturation 30min at least.Thin web placed face down behind the point sample in development chamber, is regulated placement location and expansion direction behind the glass sheet that alignment covers, developping agent launches fixing mutually by core is continual.Utilize hair dryer to dry up expansion plate behind the expansion 2-5min and carry out stratographic analysis.
The degree of separation Rs that calculates uranin and rhodamine B by fluorescence microscope is 1.89.Studies show that of this part, micro-nano structure film has certain separating effect in order, and compares with the commercialization silica gel plate, and required development distance is shorter, can reach lower detectability, and this has important meaning for further raising chromatography resolution.
Embodiment two
Adopt the St ber method of improvement, prepare the single dispersion solid silicon dioxide microsphere of particle diameter from tens nanometers to several microns.By adding surfactant control seed growth, realized the growth of monodispersity mesoporous silicon oxide shell, and finally obtained the good mesoporous silicon dioxide micro-sphere of monodispersity.Subsequently, choose particle diameter for 1um concentration is 45% meso-porous titanium dioxide colloidal silica solution, utilize vertical deposition method to prepare to have the photon crystal film of high-sequential micro-nano structure.To put into constant temperature oven behind the 2d dry with leaving standstill under 65 ℃ of the films, baking temperature control is at 105-110 ℃, about 2-3 hour drying time, after the oven dry, previously prepared polystyrene solution dripped in film surface leave standstill a period of time, make polystyrene solution be full of the gap between the silicon dioxide microsphere fully.Treat behind the film drying it is inserted in the muffle furnace and be cooled to room temperature behind 800 ℃ of calcining 4h.Utilize SEM observation, the TLC film that obtains as can be known has the counter opal structure that is modified with meso-hole structure.
By the separation of mixed dye being assessed the thin-layer chromatography effect of prepared film.Mixed dye is made up of the blue II of dimethyl yellow, Sudan IV and the Sudan, and point sample is preceding with dilution with toluene to 10
-2M, 10
-3M and 10
-4M also mixes.Utilize the blunt mouthful of glass capillary absorption～10nl potpourri of internal diameter 43um to carry out parallel point sample, point of sample interval～4mm is positioned at upper edge, film bottom～3mm place.
Chromatographic resolution is carried out in small-sized vertical expansion cylinder and homemade parallel TLC development chamber.Before launching with the toluene of 3:7 volume ratio and normal hexane is added into liquid-accumulating chamber as developping agent and conditioning chamber carries out presaturation 30min at least.Thin web placed face down behind the point sample in development chamber, is regulated placement location and expansion direction behind the glass sheet that alignment covers, developping agent launches fixing mutually by core is continual.Utilize hair dryer to dry up expansion plate behind the expansion 2-5min and carry out stratographic analysis.
Can observe blue three looks of reddish yellow very clearly by scanner separates, its medium blue-red degree of separation has reached 1.65, plate hights such as the theory of dimethyl yellow have reached 19um, show that orderly micro-nano structure film has certain separating effect, and compare with the commercialization silica gel plate, required development distance is shorter, can reach lower detectability, and this has important meaning for further raising chromatography resolution.
Claims (9)
1. chromatographic sheet with orderly micro-nano structure, comprise substrate and be arranged on fixedly phase on the described substrate, it is characterized in that: described fixing is made up of skeleton and the mesoporous microstructure of the counter opal structure with orderly micro-nano structure mutually, wherein the skeleton of counter opal structure is the template preparation with the photon crystal film, is modified with described mesoporous microstructure on the skeleton surface of counter opal structure.
2. a kind of chromatographic sheet with orderly micro-nano structure according to claim 1, it is characterized in that, the macropore diameter of counter opal structure is 200～1000nm, and photon band gap is distributed in the zone of 400～2000nm, and the aperture of mesoporous microstructure is 3～10nm.
3. according to claim 1 and 2 described a kind of chromatographic sheet with orderly micro-nano structure, it is characterized in that: photon crystal film thickness is at 10～120um.
4. a kind of chromatographic sheet with orderly micro-nano structure according to claim 3 is characterized in that: micro-nano structure is formed by single finely disseminated nano-colloid particle self assembly in order.
5. a kind of chromatographic sheet with orderly micro-nano structure according to claim 4, it is characterized in that: described colloidal particle material is silicon dioxide or polystyrene, and the colloidal particle particle diameter is between 200nm～1um; The material of substrate is silicon dioxide, aluminium oxide, low bulk high temperature borosilicate glass, steel or silicon wafer.
6. a kind of chromatographic sheet with orderly micro-nano structure according to claim 4, it is characterized in that: described single good dispersion nano-colloid particle is that inorganic nano-particle is or/and organic nano particle and their derivant, described inorganic nano-particle comprises non magnetic inorganic nano-particle and magnetic inorganic nano-particle, described non magnetic inorganic nano-particle comprises nonmagnetic metal nano particle and non magnetic nonmetal nano particle, and described derivant comprises and is combined with surface group or/and be coated with the derivant of machine thing.
7. a kind of chromatographic sheet with orderly micro-nano structure according to claim 6, it is characterized in that: described nonmagnetic metal nano particle is that silicon oxide particle, Titanium particles or aluminium oxide particles are at interior oxide nano-particles.
8. a kind of chromatographic sheet with orderly micro-nano structure according to claim 6, it is characterized in that: described metal nanoparticle is gold particle, silver particles, iron particle, palladium particle, chromium particle or nickel particles.
9. method for the manufacture of the described chromatographic sheet of claim 1 is characterized in that step is as follows:
The first step, with silicon dioxide, pipe/polyhenylethylene nano colloidal particle by gravity deposition, vertical czochralski method or directly coat at substrate and form described orderly micro-nano structure, at least part of photon crystal film with orderly micro-nano structure that forms by self assembly;
Second goes on foot, silicon dioxide, pipe/polyhenylethylene nano colloidal particle is filled and entered in the space of the photon crystal film that assembles by immersion, dropping method;
The 3rd step, with the photon crystal film that assembles as template, remove template by chemical corrosion or high-temperature calcination method, obtain the counter opal structure of periodic arrangement;
The 4th the step, on the surface of counter opal structure utilize graft polymer or depositing silicon gluing method in the photon crystal film finishing mesoporous microstructure of counter opal structure at last, and carry out Development of Thin-Layer Chromatography with this mutually as chromatographic stationary.
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| US11610509B2 (en) | 2021-01-04 | 2023-03-21 | Saudi Arabian Oil Company | Fabrication of micromodels for carbonate reservoirs |
| US11660595B2 (en) | 2021-01-04 | 2023-05-30 | Saudi Arabian Oil Company | Microfluidic chip with multiple porosity regions for reservoir modeling |
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| US11610509B2 (en) | 2021-01-04 | 2023-03-21 | Saudi Arabian Oil Company | Fabrication of micromodels for carbonate reservoirs |
| US11660595B2 (en) | 2021-01-04 | 2023-05-30 | Saudi Arabian Oil Company | Microfluidic chip with multiple porosity regions for reservoir modeling |
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| US11911761B2 (en) | 2021-01-22 | 2024-02-27 | Saudi Arabian Oil Company | Microfluidic chip with mixed porosities for reservoir modeling |
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Application publication date: 20130828 |