CN105277650A - Double-stationary-phase thin-layer chromatoplate and preparation method therefor - Google Patents
Double-stationary-phase thin-layer chromatoplate and preparation method therefor Download PDFInfo
- Publication number
- CN105277650A CN105277650A CN201510039488.3A CN201510039488A CN105277650A CN 105277650 A CN105277650 A CN 105277650A CN 201510039488 A CN201510039488 A CN 201510039488A CN 105277650 A CN105277650 A CN 105277650A
- Authority
- CN
- China
- Prior art keywords
- thin layer
- stationary liquid
- hydrophilic
- hydrophobic
- liquid thin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention provides a double-stationary-phase thin-layer chromatoplate and a preparation method therefor. The thin-layer chromatoplate comprises a base plate and a stationary phase thin layer. The chromatoplate also comprises a border line, a hydrophilic stationary phase thin layer and a hydrophobic stationary phase thin layer. The hydrophilic stationary phase thin layer and the hydrophobic stationary phase thin layer are porous, and attached at two sides of the border line on the base plate respectively, the thicknesses of the two thin layers are the same, and the two thin layers are in bonding connection at the border line. The invention also provides a preparation method for the double-stationary-phase thin-layer chromatoplate. The preparation method comprises the following steps: a hydrophilic polymer fluid and a hydrophobic polymer fluid are prepared; a hydrophilic stationary phase thin layer is prepared; part of the hydrophilic stationary phase thin layer is scraped, and a hydrophobic stationary phase thin layer is prepared at the scraped position; activation processing is carried out. The hydrophilic stationary phase thin layer and the hydrophobic stationary phase thin layer are prepared individually, mutual interference of control of pore diameters of the two thin layers is avoided, ideal pore diameters can be obtained, and therefore the separation effects of the chromatoplate are raised.
Description
Technical field
The present invention relates to a kind of two Stationary liquid chromatographic sheet and preparation method, belong to technical field of chromatography,
Background technology
Thin-layered chromatography is that the lamelliform holder of the porous structure coated on substrate is as Stationary liquid, with suitable solvent for mobile phase, utilize each composition different to same adsorbent ability, make to flow through in the process of Stationary liquid (adsorbent) in mobile phase (solvent), continuous print produce Adsorption and desorption attached, adsorb again, desorption again, thus reach the object disconnected from each other of each composition.
When Stationary liquid is the polar adsorbent of strongly hydrophilic, chromatographic sheet has hydrophilic chromatographic function, and when Stationary liquid is the non-polar adsorbent of hydrophobic nature, chromatographic sheet has hydrophobic chromatography function.Two Stationary liquid chromatographic sheet are one of chromatographic sheet, are to be incorporated on same substrate by the thin layer of two kinds of Stationary liquid, thus have two kinds of separation functions, such as, have hydrophilic chromatographic function and hydrophobic chromatography function simultaneously.The pore diameter distribution of Stationary liquid is very large on adsorptive power impact, therefore also just decides the chromatographic resolution effect of chromatographic sheet.The Stationary liquid of chromatographic sheet has three kinds of pore diameter distributions: macropore is aperture is more than 50nm, and mesopore is aperture is 50nm ~ 2nm, and micropore is aperture is below 2nm.And the ratio that diameter is in shared by the hole in mesopore range is larger, the separating effect of chromatographic sheet is better.
Polyalcohol integral material is the continuous Stationary liquid utilizing polymerization to carry out in-situ polymerization formation on substrate, has been widely used in fields such as high performance liquid chromatography, high speed affinity chromatography and Capillary Electrophoresis chromatogram, gas chromatography, liquid-solid extractions.At present, utilize polyalcohol integral material to prepare the method for two Stationary liquid chromatographic sheet to only have photo-grafting technology.Such as the preparation of when there is two Stationary liquid chromatographic sheet of hydrophilic chromatographic function and hydrophobic chromatography function simultaneously, the detailed process of photo-grafting technology is using glass plate as substrate, the hydrophilic thin layer of the porous be attached on substrate is first obtained with hydrophilic polymeric liquid, after washing away pore-foaming agent, use hydrophobic polymeric liquid this hydrophilic thin layer moistening again, then with quartz plate, thin layer is covered, cover the blindage of the not saturating ultraviolet light of white space again, after ultraviolet lighting, with dry after washed with methanol, obtain connecting hydrophobic polymers at former lamellate white space, form the hydrophobic thin film of new porous.
Photo-grafting technology belongs to the method for synthesis post-modification, and can only connect other side chains in the inside in the hole of original hydrophilic thin layer, the relatively original thin layer aperture of new hydrophobic thin film can be made to reduce, and therefore the pore diameter distribution of whole chromatographic sheet is uneven and uncontrollable.Because the chromatographic resolution effect of aperture to chromatographic sheet plays a decisive role, and aperture in Stationary liquid thin layer prepared by photo-grafting technology is uneven and uncontrollable, so be difficult to realize the good pore diameter distribution of separating effect, thus the chromatographic resolution effect of the two Stationary liquid chromatographic sheet of impact.
Summary of the invention
The object of the invention is to, a kind of two Stationary liquid chromatographic sheet that can improve chromatographic resolution effect are provided.
Another object of the present invention, provides the preparation method of a kind of pair of Stationary liquid chromatographic sheet, can prepare and have even aperture distribution and controlled two Stationary liquid thin layers, thus improves two Stationary liquid chromatographic sheet of chromatographic resolution effect.
The technical matters that will solve required for the present invention, can be achieved through the following technical solutions:
As a first aspect of the present invention, a kind of two Stationary liquid chromatographic sheet, comprise substrate and two Stationary liquid thin layer, described substrate is glass plate, described pair of Stationary liquid thin layer is porous, described pair of Stationary liquid thin layer comprises the hydrophilic Stationary liquid thin layer with hydrophilic chromatographic function and the hydrophobic Stationary liquid thin layer with hydrophobic chromatography function simultaneously, described pair of Stationary liquid thin layer depends on the substrate, it is characterized in that, described substrate is the glass plate of rectangle, the diameter in described hole is evenly distributed, described hydrophilic Stationary liquid thin layer is poly-(glycidyl methacrylate-ethylene glycol dimethacrylate) integral material, described hydrophobic Stationary liquid thin layer is poly-(butyl methacrylate-ethylene glycol dimethacrylate) integral material, described chromatosheet also comprises boundary line, described boundary line is the middle part being positioned at described substrate, upper with described substrate, that sideline, downside is intersected and be the straight line of 0 ° ~ 20 ° relative to the angle of vertical direction, described hydrophilic Stationary liquid thin layer and described hydrophobic Stationary liquid thin layer are attached on the described substrate of both sides, described boundary line respectively, both thickness is identical, connect at described boundary line place bonding, described hydrophilic Stationary liquid thin layer and the described outer ledge of hydrophobic Stationary liquid thin layer and the mean distance of described boundary line are not less than 2cm.
Of the present invention pair of Stationary liquid chromatographic sheet is further characterized in that: the thickness of hydrophilic Stationary liquid thin layer and hydrophobic Stationary liquid thin layer is 100 ~ 200 μm.
Of the present invention pair of Stationary liquid chromatographic sheet is further characterized in that: angle is 10 °.
Of the present invention pair of Stationary liquid chromatographic sheet is further characterized in that: the thickness of hydrophilic Stationary liquid thin layer and hydrophobic Stationary liquid thin layer is 100 ~ 200 μm, and angle is 10 °.
As a second aspect of the present invention, prepare above-mentioned two Stationary liquid chromatographic sheet, it is characterized in that, comprise the following steps:
Step one: preparation hydrophilic polymeric liquid and hydrophobic polymeric liquid
By the first monomer, first crosslinking chemical, first pore-foaming agent and the first initiating agent are mixed to get hydrophilic polymeric liquid, first monomer is glycidyl methacrylate, first crosslinking chemical is ethylene glycol dimethacrylate, first pore-foaming agent is cyclohexanol, first initiating agent is 2-hydroxy-2-methyl propiophenone, glycidyl methacrylate: ethylene glycol dimethacrylate: the mass ratio of cyclohexanol is 0.24:0.16:0.60, 2-hydroxy-2-methyl propiophenone is 0.01:1 with glycidyl methacrylate and ethylene glycol dimethacrylate mixture quality ratio, by second comonomer, second crosslinking chemical, second pore-foaming agent and the second initiating agent are mixed to get hydrophobic polymeric liquid, second comonomer is butyl methacrylate, second crosslinking chemical is ethylene glycol dimethacrylate, second pore-foaming agent is cyclohexanol and 1-4 butylene glycol, second initiating agent is benzoin methyl ether, butyl methacrylate: ethylene glycol dimethacrylate: cyclohexanol: 1-4 butylene glycol mass ratio is 0.24:0.16:0.41:0.19, benzoin methyl ether is 0.01:1 with butyl methacrylate and ethylene glycol dimethacrylate mixture quality ratio,
Step 2: prepare hydrophilic Stationary liquid thin layer
First the both sides between two pieces of glass plates are encased inside filter paper bar, clamp two pieces of glass plates and make mould, hydrophilic polymeric liquid is immersed with standing manner in its one end by mould, hydrophilic polymeric liquid fills the inner space of mould under capillary action, then mould is placed in the 1cm ~ 1.5cm place under uviol lamp, irradiate 25min ~ 35min, the wavelength of ultraviolet light is 254nm, impel hydrophilic polymeric liquid to carry out polyreaction in mould, between two pieces of glass plates, form hydrophilic Stationary liquid thin layer;
Step 3: prepare hydrophobic Stationary liquid thin layer
Remove mould, the glass plate of the side of taking off is as substrate, and boundary line is marked on substrate, strike off the hydrophilic Stationary liquid thin layer of substrate upper border line side, and be encased inside filter paper bar by the both sides of substrate and boundary line, another block glass plate is covered on substrate, mould made by clamping glass plate and substrate, blank end toward mould slowly injects hydrophobic polymeric liquid, hydrophobic polymeric liquid fills the inner space of mould under capillary action, then under mould being placed in uviol lamp, 25min ~ 35min is irradiated at 1cm ~ 1.5cm place, the wavelength of ultraviolet light is 254nm, hydrophobic polymeric liquid is impelled to carry out polyreaction in mould, hydrophobic Stationary liquid thin layer is formed between glass plate and substrate, simultaneously, hydrophobic Stationary liquid thin layer is connected at boundary line place bonding with hydrophilic Stationary liquid thin layer, the two Stationary liquid thin layer of both compositions one, be attached on substrate,
Step 4: activation process
Remove described mould, the described substrate depending on described pair of Stationary liquid thin layer is immersed process 6 ~ 12h in methyl alcohol or ethanol, take out, after drying, immersing concentration is the H of 0.3 ~ 0.6mol/L
2sO
4in solution, water bath processing 2 ~ 3h at 50 ~ 80 DEG C, takes out, and rinses, after drying, obtains described pair of Stationary liquid chromatographic sheet.
The preparation method of of the present invention pair of Stationary liquid chromatographic sheet is further characterized in that: in step 2, two pieces of glass plates are before use through silanization pretreatment.
The preparation method of of the present invention pair of Stationary liquid chromatographic sheet is further characterized in that: in step 2 and step 3, uviol lamp is double, and the power of the uviol lamp often arranged is 8w.
The preparation method of of the present invention pair of Stationary liquid chromatographic sheet is further characterized in that: in step 2, two blocks of glass sheet are before use through silanization pretreatment, and in step 2 and step 3, uviol lamp is double, and the power of the uviol lamp often arranged is 8w.
Invention effect and effect
According to the preparation method of of the present invention pair of Stationary liquid chromatographic sheet, boundary line is marked owing to prepare hydrophilic Stationary liquid thin layer on substrate after, and strike off the hydrophilic Stationary liquid thin layer of side, boundary line, then at the hydrophobic Stationary liquid thin layer of the place's of striking off preparation, and hydrophobic Stationary liquid thin layer is connected with hydrophilic Stationary liquid thin layer bonding at boundary line place, make both be attached on the substrate of both sides, boundary line respectively, the two Stationary liquid thin layer of composition, thus obtain two Stationary liquid chromatographic sheet; And prepare separately in both sides, boundary line due to hydrophilic Stationary liquid thin layer of the present invention and hydrophobic Stationary liquid thin layer, the control in both apertures can not be interfered with each other, more preferably aperture can be obtained, thus the separating effect of chromatographic sheet can be improved.
According to of the present invention pair of Stationary liquid chromatographic sheet, because hydrophilic Stationary liquid thin layer and hydrophobic Stationary liquid thin layer prepare separately, the uniform pore diameter of the two Stationary liquid thin layers therefore formed and controlled, instead of in picture prior art, connect side chain in inside, former lamellate hole, therefore the present invention can obtain more preferably pore diameter distribution, and the uniform diameter in hole is distributed, and diameter to be in the ratio that the hole in mesopore range accounts for maximum, thus improve chromatographic resolution effect.
Accompanying drawing explanation
Fig. 1 is of the present invention pair of Stationary liquid chromatographic sheet structural representation in an embodiment; And
Fig. 2 is the effect schematic diagram of of the present invention pair of Stationary liquid chromatographic sheet for chromatographic resolution.
Embodiment
Below in conjunction with concrete case study on implementation, technical scheme of the present invention is described further.
Fig. 1 is of the present invention pair of Stationary liquid chromatographic sheet structural representation in an embodiment.
As shown in Figure 1, two Stationary liquid chromatographic sheet 10 two Stationary liquid thin layers of comprising substrate and being formed on substrate.
Substrate is the glass plate of rectangle, and specifically length is 7cm, width is the microslide of 2.6cm.The center score of substrate has the boundary line 3 crossing with upper and lower sides sideline, and the angle in opposed vertical direction, boundary line 3 is 10 °.Two Stationary liquid thin layer be porous structure, be attached on substrate.The thickness of two Stationary liquid thin layer is 100 μm.The thickness of the two Stationary liquid thin layers in certain the present embodiment can also be other numerical value in 100 ~ 200 μm.
Two Stationary liquid thin layer comprises the hydrophilic Stationary liquid thin layer 1 with hydrophilic chromatographic function and the hydrophobic Stationary liquid thin layer 2 with hydrophobic chromatography function.The composition of hydrophilic Stationary liquid thin layer 1 is poly-(glycidyl methacrylate-ethylene glycol dimethacrylate) integral material.The composition of hydrophobic Stationary liquid thin layer 2 is poly-(butyl methacrylate-ethylene glycol dimethacrylate) integral material.
As shown in Figure 1, hydrophilic Stationary liquid thin layer 1 is positioned at the left side of substrate, and hydrophobic Stationary liquid thin layer 2 is positioned at the right side of substrate.Hydrophilic Stationary liquid thin layer 1 and hydrophobic Stationary liquid thin layer 2 are porous, and the substrate being attached to both sides, boundary line 3 respectively connects at boundary line 3 place bonding,
In the present embodiment, the uniform pore diameter distribution of hydrophilic Stationary liquid thin layer 1 and hydrophobic Stationary liquid thin layer 2, and diameter to be distributed in the ratio that the hole in mesopore range accounts for maximum, be optimal pore diameter distribution, therefore two Stationary liquid chromatographic sheet separating effects of the present embodiment are very good.
Fig. 2 is the effect schematic diagram of of the present invention pair of Stationary liquid chromatographic sheet for chromatographic resolution.
By Stationary liquid chromatographic sheet 10 two in Fig. 1 for separating of 4 kinds of dyestuffs.In hydrophobic Stationary liquid thin layer 2, select the mixed liquor of 4 kinds of dyestuffs from 1cm place, boundary line, point sample place is apart from the coboundary 0.5cm of hydrophobic Stationary liquid thin layer 2.In figure, vertical dotted line is the first dimension detaching direction, arrow points developping agent flow direction.Horizontal dotted line is for being the second dimension detaching direction, arrow points agent flow direction.
Mixed liquor is bone dry after the first dimension is launched, and obtains the result as shown in Fig. 2 (a).As we know from the figure, three spots are had after separation.Hydrophobic Stationary liquid thin layer 2 has hydrophobic chromatography function, and the methyl red that therefore polarity is less and P-aminoazobenzene are separated in hydrophobic Stationary liquid thin layer 2, form two spots respectively in the below of hydrophobic Stationary liquid thin layer 2.And the larger R6G of polarity is not separated with malachite green, form mixed dot.
Then by mixed dot to two-dimensional development.In order to avoid the spot of separator well is destroyed, adopt filter paper bar to launch, immerse developping agent by one of filter paper bar section, the other end is attached to the edge of mixed dot, be sent in hydrophilic Stationary liquid thin layer 1, and obtained the result as shown in Fig. 2 (b) after launching separation.Hydrophilic Stationary liquid thin layer 1 has hydrophilic chromatographic function, and the R6G that therefore polarity is larger is separated in hydrophilic Stationary liquid thin layer 1 with malachite green, forms two spots.
As can be seen from Figure 2, utilize the two Stationary liquid chromatographic sheet in the present embodiment, 4 kinds of dyestuffs can be separated completely, separating effect is fine, illustrate that the two Stationary liquid chromatographic sheet in the present embodiment have hydrophilic chromatographic function and hydrophobic chromatography function simultaneously, and separating effect is fine.
Wherein, boundary line 3 is arranged to 10 °, has certain inclination angle, is to make mixed dot distance border comparatively near, being more easily extended in hydrophilic Stationary liquid thin layer 1, and can not affect should the spot of methyl red through separating and P-aminoazobenzene.The inclination angle of the boundary line 3 of certain the present embodiment also can according to the actual needs of material to be separated, and that is arranged in 0 ° ~ 20 ° is arbitrarily angled.
The outer ledge of hydrophilic Stationary liquid thin layer 1 and hydrophobic Stationary liquid thin layer 2 and the mean distance at least 2cm of boundary line 3, be to ensure that developping agent can have enough flowing spaces in hydrophilic Stationary liquid thin layer 1 and hydrophobic Stationary liquid thin layer 2, the material to be separated mass-energy be dissolved in wherein is separated.If the distance of Edge Distance boundary line 3 is too small, expansion can be caused insufficient, and material can not be effectively separated.
The preparation method of the two Stationary liquid chromatographic sheet adopted in the present embodiment, can prepare above-mentioned two Stationary liquid chromatographic sheet 10, comprise the following steps:
(1) silanization treatment substrate
Get two pieces of microslides as shown in fig. 1, after using water and alcohol flushing successively, immerse 30min in the NaOH solution of 0.5mol/L, make slide surface modify upper hydroxyl; Wash with water after taking-up, then 30min in the HCl aqueous solution immersing 0.5mol/L, hydroxyl is fully exposed; By microslide dry 1h at 60 DEG C, immerse after cooling in the ethanolic solution of 3-(isobutylene acyl-oxygen) the oxypropyl trimethyl silane of 20% (v/v) and spend the night, make microslide alkylation; Taking-up is dewatered at being placed on 35 DEG C 1.5h, finally the microslide handled well is placed in dark place and preserves.
(2) hydrophilic polymeric liquid and hydrophobic polymeric liquid is prepared
Choose glycidyl methacrylate as the first monomer, take 1.92g; Choose ethylene glycol dimethacrylate as the first crosslinking chemical, take 1.28g; Choose cyclohexanol as the first pore-foaming agent, take 4.8g; Choose 2-hydroxy-2-methyl propiophenone as the first initiating agent, take 0.032g; After mentioned reagent being mixed, ultrasonic 15min makes it fully mix and degasification, obtains hydrophilic polymeric liquid.
Choose butyl methacrylate and do second for monomer, take 1.92g; Choose ethylene glycol dimethacrylate as the second crosslinking chemical, take 1.28g; Choose cyclohexanol and 1-4 butylene glycol as the second pore-foaming agent, take cyclohexanol 4.8g, take 1-4 butylene glycol 1.52g; Choose benzoin methyl ether as the second initiating agent, take 0.032g; After mentioned reagent being mixed, ultrasonic 15min makes it fully mix and degasification, obtains hydrophobic polymeric liquid.
(3) hydrophilic Stationary liquid thin layer is prepared
Be encased inside two filter paper bars in the middle of microslide after two pieces of activation, two filter paper bars are distributed in the both sides of microslide, make simple mould by clamp.Hydrophilic polymeric liquid is immersed with standing manner in its one end by mould, and hydrophilic polymeric liquid can fill the inner space of mould under capillary action, infiltrates the other end of microslide.
Irradiate 30min under mould being placed in double uviol lamp in fuming cupboard, uviol lamp lies in a horizontal plane in 1.2cm place above mould, and the power of uviol lamp is 8w, and wavelength is 254nm.Hydrophilic polymeric liquid carries out polyreaction on microslide, generates poly-(glycidyl methacrylate-ethylene glycol dimethacrylate) integral material, thus forms hydrophilic Stationary liquid thin layer 1.In fuming cupboard, carry out polyreaction, good heat radiation can be reached, eliminate the impact of temperature on polymerization.Now, the side chain of hydrophilic Stationary liquid thin layer 1 is hydrophobic epoxy radicals, and therefore, hydrophilic Stationary liquid thin layer 1 now shows hydrophobicity.
(4) hydrophobic Stationary liquid thin layer is prepared
Remove mould, the microslide of the side of taking off, as substrate, and thereon by marking boundary line 3 shown in Fig. 1.Then, strike off hydrophilic Stationary liquid thin layer 1 with pocket knife in side, boundary line 3, and be again encased inside two filter paper bars in the region of striking off.Refitting mould, with syringe toward slowly being injected hydrophobic polymeric liquid by the blank end striking off hydrophilic Stationary liquid thin layer 1, makes the stripping areas in hydrophobic polymeric liquid filling mould.New filter paper bar needs the both sides and the boundary line 3 that are close to substrate, prevents hydrophobic polymeric liquid from penetrating into the centre of hydrophilic Stationary liquid thin layer 1.
Irradiate 30min under mould being placed in double uviol lamp in fuming cupboard, uviol lamp lies in a horizontal plane in 1.2cm place above mould, and the power of uviol lamp is 8w, and wavelength is 254nm.Hydrophobic polymeric liquid carries out polyreaction on substrate, generates poly-(butyl methacrylate-ethylene glycol dimethacrylate) integral material, thus forms hydrophobic Stationary liquid thin layer 2.Now, the side chain of hydrophobic Stationary liquid thin layer 2 is hydrophobic butyl, and therefore hydrophobic Stationary liquid thin layer 2 is hydrophobicity, has hydrophobic chromatography function.
Meanwhile, hydrophilic Stationary liquid thin layer 1 and hydrophobic Stationary liquid thin layer 2, at boundary line 3 place bonding, link together by the edge of hydrophobic polymeric liquid and hydrophilic Stationary liquid thin layer 1.This is because hydrophilic polymeric liquid carries out after polyreaction forms hydrophilic Stationary liquid thin layer 1, residual a part of hydrophilic polymeric liquid is also had in hydrophilic Stationary liquid thin layer 1, some first monomers are not polymerized completely with the first crosslinking chemical, and the group come out in addition, so hydrophobic polymeric liquid still can form covalent bond with the edge of hydrophilic Stationary liquid thin layer 1, thus be bonded together.And slowly injecting mould due to hydrophobic polymeric liquid, the hydrophobic polymeric liquid therefore injected to penetrate in the middle of the hydrophilic Stationary liquid thin layer 1 that has been polymerized, the just edge contact of hydrophilic Stationary liquid thin layer 1.
Therefore, hydrophilic Stationary liquid thin layer 1 is connected at boundary line 3 place bonding with hydrophobic Stationary liquid thin layer 2, and both form a two Stationary liquid thin layer, are attached on substrate.
(5) activation process
Again remove mould, attached lamellate substrate is immersed in ethanol and processes 12h, get rid of the pore-foaming agent in hydrophilic Stationary liquid thin layer 1 and hydrophobic Stationary liquid thin layer 2, and unreacted monomer and crosslinking chemical.Attached lamellate substrate is taken out from ethanol, at room temperature dry.
Immerse the H of 0.5mol/L
2sO
4in aqueous solution, 60 DEG C of water bath processing 3h.Before utilizing sulfuric acid treatment, the side chain of hydrophilic Stationary liquid thin layer 1 is hydrophobicity epoxy radicals, shows hydrophobicity, but sulfuric acid treatment can make epoxy ring-opening form o-dihydroxy, water wettability strengthens greatly, thus makes hydrophilic Stationary liquid thin layer 1 show water wettability, thus possesses the function of hydrophilic chromatographic.Now, two Stationary liquid thin layer has hydrophilic chromatographic function and hydrophobic chromatography function simultaneously.
Then the substrate with two Stationary liquid thin layer is taken out, by a large amount of water and ethanol rinse extremely neutrality, and be placed in 40 DEG C of dryings; Thus obtaining two Stationary liquid chromatographic sheet 10, this pair of Stationary liquid chromatographic sheet has hydrophobic chromatography and hydrophilic chromatographic two kinds of functions.
Embodiment effect and effect
According to the preparation method of two Stationary liquid chromatographic sheet of the present embodiment, boundary line is marked owing to prepare hydrophilic Stationary liquid thin layer on substrate after, and strike off the hydrophilic Stationary liquid thin layer of side, boundary line, then at the hydrophobic Stationary liquid thin layer of the place's of striking off preparation, and hydrophobic Stationary liquid thin layer is connected with hydrophilic Stationary liquid thin layer bonding at boundary line place, make both be attached on the substrate of both sides, boundary line respectively, the two Stationary liquid thin layer of composition, thus obtain two Stationary liquid chromatographic sheet; And prepare separately in both sides, boundary line due to hydrophilic Stationary liquid thin layer of the present invention and hydrophobic Stationary liquid thin layer, the control in both apertures can not be interfered with each other, more preferably aperture can be obtained, thus the separating effect of chromatographic sheet can be improved.
According to of the present invention pair of Stationary liquid chromatographic sheet, because hydrophilic Stationary liquid thin layer and hydrophobic Stationary liquid thin layer prepare separately, the uniform pore diameter of the two Stationary liquid thin layers therefore formed and controlled, instead of in picture prior art, connect side chain in inside, former lamellate hole, therefore the present invention can obtain more preferably pore diameter distribution, and the uniform diameter in hole is distributed, and diameter to be in the ratio that the hole in mesopore range accounts for maximum, thus improve chromatographic resolution effect.
Certain technical scheme of the present invention is not limited in the description in above embodiment.Irradiation time under uviol lamp can also be selected arbitrarily in 25min ~ 35min.With the H that the substrate of two Stationary liquid thin layer can also immerse
2sO
4the concentration of aqueous solution can also be selected arbitrarily in 0.3 ~ 0.6mol/L, and the temperature of water bath processing can also be selected arbitrarily in 50 ~ 80 DEG C, and the time of water bath processing can also be selected arbitrarily in 2 ~ 3h.Substrate with two Stationary liquid thin layer can also immerse in methyl alcohol and process, and the processing time can also be selected arbitrarily in 6 ~ 12h.
Claims (8)
1. a two Stationary liquid chromatographic sheet, comprise substrate and two Stationary liquid thin layer, described substrate is glass plate, described pair of Stationary liquid thin layer is porous, described pair of Stationary liquid thin layer comprises the hydrophilic Stationary liquid thin layer with hydrophilic chromatographic function and the hydrophobic Stationary liquid thin layer with hydrophobic chromatography function simultaneously, described pair of Stationary liquid thin layer depends on the substrate, it is characterized in that, described substrate is the glass plate of rectangle, the diameter in described hole is evenly distributed, described hydrophilic Stationary liquid thin layer is poly-(glycidyl methacrylate-ethylene glycol dimethacrylate) integral material, described hydrophobic Stationary liquid thin layer is poly-(butyl methacrylate-ethylene glycol dimethacrylate) integral material, described chromatosheet also comprises boundary line, described boundary line is the middle part being positioned at described substrate, upper with described substrate, that sideline, downside is intersected and be the straight line of 0 ° ~ 20 ° relative to the angle of vertical direction, described hydrophilic Stationary liquid thin layer and described hydrophobic Stationary liquid thin layer are attached on the described substrate of both sides, described boundary line respectively, both thickness is identical, connect at described boundary line place bonding, described hydrophilic Stationary liquid thin layer and the described outer ledge of hydrophobic Stationary liquid thin layer and the mean distance of described boundary line are not less than 2cm.
2. according to claim 1 pair of Stationary liquid chromatographic sheet, is characterized in that, the thickness of described hydrophilic Stationary liquid thin layer and described hydrophobic Stationary liquid thin layer is 100 ~ 200 μm.
3. according to claim 1 pair of Stationary liquid chromatographic sheet, is characterized in that, described angle is 10 °.
4. according to claim 1 pair of Stationary liquid chromatographic sheet, is characterized in that, the thickness of described hydrophilic Stationary liquid thin layer and described hydrophobic Stationary liquid thin layer is 100 ~ 200 μm, and described angle is 10 °.
5. a preparation method for two Stationary liquid chromatographic sheet described in claim 1, is characterized in that, comprise the following steps:
Step one: preparation hydrophilic polymeric liquid and hydrophobic polymeric liquid
By the first monomer, first crosslinking chemical, first pore-foaming agent and the first initiating agent are mixed to get described hydrophilic polymeric liquid, first monomer is glycidyl methacrylate, first crosslinking chemical is ethylene glycol dimethacrylate, first pore-foaming agent is cyclohexanol, first initiating agent is 2-hydroxy-2-methyl propiophenone, glycidyl methacrylate: ethylene glycol dimethacrylate: the mass ratio of cyclohexanol is 0.24:0.16:0.60, 2-hydroxy-2-methyl propiophenone is 0.01:1 with glycidyl methacrylate and ethylene glycol dimethacrylate mixture quality ratio, by second comonomer, second crosslinking chemical, second pore-foaming agent and the second initiating agent are mixed to get described hydrophobic polymeric liquid, second comonomer is butyl methacrylate, second crosslinking chemical is ethylene glycol dimethacrylate, second pore-foaming agent is cyclohexanol and 1-4 butylene glycol, second initiating agent is benzoin methyl ether, butyl methacrylate: ethylene glycol dimethacrylate: cyclohexanol: 1-4 butylene glycol mass ratio is 0.24:0.16:0.41:0.19, benzoin methyl ether is 0.01:1 with butyl methacrylate and ethylene glycol dimethacrylate mixture quality ratio,
Step 2: prepare hydrophilic Stationary liquid thin layer
First the both sides between two pieces of glass plates are encased inside filter paper bar, clamp two pieces of glass plates and make mould, described hydrophilic polymeric liquid is immersed with standing manner in its one end by described mould, described hydrophilic polymeric liquid fills the inner space of described mould under capillary action, then described mould is placed in the 1cm ~ 1.5cm place under uviol lamp, irradiate 25min ~ 35min, the wavelength of ultraviolet light is 254nm, impel described hydrophilic polymeric liquid to carry out polyreaction in described mould, between described two pieces of glass plates, form described hydrophilic Stationary liquid thin layer;
Step 3: prepare hydrophobic Stationary liquid thin layer
Remove described mould, the described glass plate of the side of taking off is as described substrate, and mark described boundary line on the substrate, strike off the hydrophilic Stationary liquid thin layer of side, described boundary line on described substrate, and be encased inside filter paper bar by the both sides of described substrate and described boundary line, another block glass plate is covered on the substrate, clamp described glass plate and mould made by described substrate, blank end toward described mould slowly injects described hydrophobic polymeric liquid, described hydrophobic polymeric liquid fills the inner space of described mould, then under described mould being placed in uviol lamp, 25min ~ 35min is irradiated at 1cm ~ 1.5cm place, the wavelength of ultraviolet light is 254nm, described hydrophobic polymeric liquid is impelled to carry out polyreaction in described mould, described hydrophobic Stationary liquid thin layer is formed between described glass plate and described substrate, simultaneously, described hydrophobic Stationary liquid thin layer is connected at described boundary line place bonding with described hydrophilic Stationary liquid thin layer, the two Stationary liquid thin layer of both compositions one, depend on the substrate,
Step 4: activation process
Remove described mould, the described substrate depending on described pair of Stationary liquid thin layer is immersed process 6 ~ 12h in methyl alcohol or ethanol, take out, after drying, immersing concentration is the H of 0.3 ~ 0.6mol/L
2sO
4in solution, water bath processing 2 ~ 3h at 50 ~ 80 DEG C, takes out, and rinses, after drying, obtains described pair of Stationary liquid chromatographic sheet.
6. the preparation method of according to claim 5 pair of Stationary liquid chromatographic sheet, is characterized in that, in described step 2, two pieces of glass plates are before use through silanization pretreatment.
7. the preparation method of according to claim 5 pair of Stationary liquid chromatographic sheet, is characterized in that, in described step 2 and step 3, described uviol lamp is double, and the power of the described uviol lamp often arranged is 8w.
8. the preparation method of according to claim 5 pair of Stationary liquid chromatographic sheet, it is characterized in that, in described step 2, two blocks of glass sheet are before use through silanization pretreatment, in described step 2 and step 3, described uviol lamp is double, and the power of the described uviol lamp often arranged is 8w.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510039488.3A CN105277650B (en) | 2015-01-26 | 2015-01-26 | A kind of pair of fixing phase chromatographic sheet and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510039488.3A CN105277650B (en) | 2015-01-26 | 2015-01-26 | A kind of pair of fixing phase chromatographic sheet and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105277650A true CN105277650A (en) | 2016-01-27 |
| CN105277650B CN105277650B (en) | 2017-03-08 |
Family
ID=55147020
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510039488.3A Active CN105277650B (en) | 2015-01-26 | 2015-01-26 | A kind of pair of fixing phase chromatographic sheet and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105277650B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109313172A (en) * | 2016-12-26 | 2019-02-05 | 松下知识产权经营株式会社 | Chromatographic sheet and used its sample analysis method |
| CN109564203A (en) * | 2016-12-26 | 2019-04-02 | 松下知识产权经营株式会社 | Chromatographic sheet and the sample analyzing method for using it |
| CN112748212A (en) * | 2019-10-31 | 2021-05-04 | 中国石油化工股份有限公司 | Method for analyzing wax content in crude oil |
| CN115166127A (en) * | 2022-07-26 | 2022-10-11 | 吉首大学 | Thin layer identification method from complex two-dimensional to simple one-dimensional |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4313906A (en) * | 1979-08-17 | 1982-02-02 | Whatman, Inc. | Two dimensional two phase thin layer chromatography plate and method |
| US20050274662A1 (en) * | 2002-06-26 | 2005-12-15 | Teledyne Isco, Inc. | Disposable monolithic column |
| CN102472733A (en) * | 2009-07-01 | 2012-05-23 | 杨百翰大学 | Thin layer chromatography plates and related methods |
| CN103026224A (en) * | 2010-05-27 | 2013-04-03 | 株式会社大赛璐 | Sample detection method by thin-layer chromatography, thin-layer chromatography plate, and method for producing same |
-
2015
- 2015-01-26 CN CN201510039488.3A patent/CN105277650B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4313906A (en) * | 1979-08-17 | 1982-02-02 | Whatman, Inc. | Two dimensional two phase thin layer chromatography plate and method |
| US20050274662A1 (en) * | 2002-06-26 | 2005-12-15 | Teledyne Isco, Inc. | Disposable monolithic column |
| CN102472733A (en) * | 2009-07-01 | 2012-05-23 | 杨百翰大学 | Thin layer chromatography plates and related methods |
| CN103026224A (en) * | 2010-05-27 | 2013-04-03 | 株式会社大赛璐 | Sample detection method by thin-layer chromatography, thin-layer chromatography plate, and method for producing same |
Non-Patent Citations (4)
| Title |
|---|
| E.F. MAKSIMOVA ET AL: "Methacrylate-based monolithic layers for planar chromatography of polymers", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| IVA URBANOVA ET AL: "Monolithic polymer layer with gradient of hydrophobicity for separation of peptides using two-dimensional thin layer chromatography and MALDI-TOF-MS detection", 《J. SEP. SCI.》 * |
| JUNSHENG S. LI ET AL: "Printable Superhydrophilic−Superhydrophobic Micropatterns Based on Supported Lipid Layers", 《LANGMUIR》 * |
| YEHUA HAN ET AL: "Monolithic Superhydrophobic Polymer Layer with Photopatterned Virtual Channel for the Separation of Peptides Using Two-Dimensional Thin Layer Chromatography-Desorption Electrospray Ionization Mass Spectrometry", 《ANALYTICAL CHEMISTRY》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109313172A (en) * | 2016-12-26 | 2019-02-05 | 松下知识产权经营株式会社 | Chromatographic sheet and used its sample analysis method |
| CN109564203A (en) * | 2016-12-26 | 2019-04-02 | 松下知识产权经营株式会社 | Chromatographic sheet and the sample analyzing method for using it |
| CN112748212A (en) * | 2019-10-31 | 2021-05-04 | 中国石油化工股份有限公司 | Method for analyzing wax content in crude oil |
| CN115166127A (en) * | 2022-07-26 | 2022-10-11 | 吉首大学 | Thin layer identification method from complex two-dimensional to simple one-dimensional |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105277650B (en) | 2017-03-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105277650A (en) | Double-stationary-phase thin-layer chromatoplate and preparation method therefor | |
| CN103446897B (en) | Chemical and ionic cross-linked alginate hydrogel flat membrane for filtration and preparation method thereof | |
| CN1170620C (en) | Polysulfone copolymer membranes and preparing process thereof | |
| US6887384B1 (en) | Monolithic microfluidic concentrators and mixers | |
| CN102580560B (en) | Method for preparing nano-material-doped polymer film | |
| Stachowiak et al. | Hydrophilic surface modification of cyclic olefin copolymer microfluidic chips using sequential photografting | |
| CN101384376A (en) | Method for producing functional membrane | |
| JP6896642B2 (en) | How to remove water from asymmetric composite membranes and feed streams | |
| CN101598717A (en) | Mould the method that legal system is equipped with polydimethylsiloxanechip chip based on the liquid of hydrogel planar micro-patterning | |
| JP2010189663A (en) | Spatially-controlled modified porous membrane | |
| CN203002392U (en) | Solid-phase extraction microfluidic analysis chip | |
| CN103709434A (en) | Preparation method and application of arteannuin molecularly imprinted membrane | |
| JP2007014854A (en) | Filtration filter, manufacturing method of filtration filter, and hemofiltration method | |
| CN105498871A (en) | Three-dimensional focusing microfluid chip and manufacturing method thereof | |
| CN1799682A (en) | Method for improving hydrophilicity of polymer porous membrane by dentritic branching molecule | |
| US20220080367A1 (en) | Efficient antifouling and hydrophilic polyethersulfone ultrafiltration membrane and preparation method thereof | |
| Lv et al. | Porous polymer-based monolithic layers enabling pH triggered switching between superhydrophobic and superhydrophilic properties | |
| JP2000042402A (en) | Liquid transport device and its production | |
| CN106179540A (en) | A kind of polymer microcontroller chip and solvent auxiliary thermal bonding method thereof | |
| Jo et al. | Microfluidic channels fabricated on mesoporous electrospun fiber mats: A facile route to microfluidic chips | |
| CN107474254B (en) | Preparation and application of organic-inorganic hydrophilic hybrid monolithic material | |
| CN105833732A (en) | Separation membrane modified by hydrophilic antifouling gel coating and preparation method thereof | |
| CN1865924A (en) | Method for making micro-fluidic chip with Z-shape spectrophotometric detection cell | |
| CN104594037A (en) | Method for preparing graft polypropylene non-woven fabric-based ion-exchange material | |
| CN111362350A (en) | Hydrophobic metal net, preparation method and application in oil-water separation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |