CN105277650B - A kind of pair of fixing phase chromatographic sheet and preparation method thereof - Google Patents
A kind of pair of fixing phase chromatographic sheet and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of pair of fixing phase chromatographic sheet, including substrate and fixing phase thin layer, chromatosheet also includes boundary line, hydrophilic fixing phase thin layer and hydrophobic fixing phase thin layer, hydrophilic fixing phase thin layer and hydrophobic fixing phase thin layer are porous, it is attached to respectively on the substrate of boundary line both sides, both thickness are identical, and at boundary line, bonding connects.The present invention also provides the preparation method of a kind of pair of fixing phase chromatographic sheet, comprises the following steps：Prepare hydrophilic polymeric liquid and hydrophobic polymeric liquid；Prepare hydrophilic fixing phase thin layer；Strike off a part of hydrophilic fixing phase thin layer, prepare hydrophobic fixing phase thin layer at the place of striking off；Activation processing.The hydrophilic fixing phase thin layer of the present invention and hydrophobic fixing phase thin layer are manufactured separately, and will not interfere with each other the control in both apertures, can obtain more preferably aperture, thus improve the separating effect of chromatosheet.
Description
Technical field
The present invention relates to a kind of pair of fixing phase chromatographic sheet and preparation method, belong to technical field of chromatography,
Background technology
Thin layer chromatography is to coat the lamelliform holder of the loose structure on substrate as fixing phase, with suitable
Solvent is mobile phase, different to same adsorbent absorbability using each composition, makes to flow through fixing phase (suction in mobile phase (solvent)
Attached dose) during, continuous produce that Adsorption and desorption is attached, adsorb again, desorption again, thus reaching the disconnected from each other of each composition
Purpose.
When fixing phase is the polar adsorbent of strongly hydrophilic, chromatographic sheet has hydrophilic chromatographic function, when fixing phase is
During the non-polar adsorbent of hydrophobicity, chromatographic sheet has hydrophobic chromatography function.Double fixing phase chromatographic sheets are thin layer colors
One kind of spectrum plate, is that the thin layer of two kinds of fixing phases is incorporated on same substrate, thus having two kinds of separation functions, for example same
When there is hydrophilic chromatographic function and hydrophobic chromatography function.The pore-size distribution of fixing phase is very big on absorbability impact, therefore also
Decide the chromatographic isolation effect of chromatographic sheet.The fixing phase of chromatographic sheet has three kinds of pore-size distributions：Macropore is that aperture is
More than 50nm, mesopore is aperture is 50nm～2nm, and micropore is aperture is below 2nm.And, diameter is in mesopore range
Ratio shared by hole is bigger, and the separating effect of chromatographic sheet is better.
Polymer integral material is the continuous fixing phase carrying out in-situ polymerization formation using polymerization on substrate, by
It is widely used in high performance liquid chromatography, high speed affinity chromatography and the field such as capillary electrophoresis chromatograph, gas chromatogram, liquid-solid extraction.
At present, the method preparing double fixing phase chromatographic sheets using polymer integral material only has photo-grafting technology.For example it is used for
When preparation has double fixing phase chromatographic sheet of hydrophilic chromatographic function and hydrophobic chromatography function simultaneously, photo-grafting technology concrete
Process is using glass plate as substrate, the hydrophilic thin layer of the porous that be attached to substrate on is first obtained with hydrophilic polymeric liquid, washes away cause
After the agent of hole, then moisten this hydrophilic thin layer with hydrophobic polymeric liquid, then with quartz plate, thin layer is covered, then cover white space
The blindage of impermeable ultraviolet light, after ultraviolet lighting, is dried after being cleaned with methanol, obtains connecting in former lamellate white space hydrophobic
Polymer, forms the hydrophobic thin film of new porous.
The method that photo-grafting technology belongs to synthesis post-modification, can only connect other in the inside in the hole of original hydrophilic thin layer
Side chain, can make the relatively original thin layer aperture of new hydrophobic thin film reduce, and the pore-size distribution of therefore whole chromatographic sheet is uneven
Even and uncontrollable.Because aperture plays a decisive role to the chromatographic isolation effect of chromatographic sheet, and photo-grafting technology preparation consolidate
The aperture determined in phase thin layer is uneven and uncontrollable, then the preferable pore-size distribution of separating effect difficult to realize, thus impact is double
The chromatographic isolation effect of fixing phase chromatographic sheet.
Content of the invention
It is an object of the invention to, a kind of double fixing phase chromatographic sheets that can improve chromatographic isolation effect are provided.
Another object of the present invention, provides the preparation method of a kind of pair of fixing phase chromatographic sheet, can prepare and have
Even aperture distribution and controlled double fixing phase thin layers, thus improve double fixing phase chromatographic sheets of chromatographic isolation effect.
The technical problem solving required for the present invention, can be achieved through the following technical solutions：
As a first aspect of the present invention, a kind of pair of fixing phase chromatographic sheet, including substrate and double fixing phase thin layer, institute
Stating substrate is glass plate, and described pair of fixing phase thin layer is porous, and described pair of fixing phase thin layer is included with hydrophilic chromatographic simultaneously
The hydrophilic fixing phase thin layer of function and the hydrophobic fixing phase thin layer with hydrophobic chromatography function, described pair of fixing phase thin layer is attached to
It is characterised in that described substrate is the glass plate of rectangle on described substrate, the diameter Distribution in described hole is uniformly, described hydrophilic solid
Determining phase thin layer is poly- (glycidyl methacrylate-ethylene glycol dimethacrylate) integral material, described hydrophobic fixation
Phase thin layer is poly- (butyl methacrylate-ethylene glycol dimethacrylate) integral material, and described chromatosheet also includes border
Line, described boundary line be intersect with the upper and lower side line of described substrate positioned at the middle part of described substrate and with respect to vertical side
To angle be 0 °～20 ° of straight line, described hydrophilic fixing phase thin layer and described hydrophobic fixing phase thin layer are attached to described respectively
On the described substrate of boundary line both sides, both thickness are identical, and at described boundary line, bonding connects, described hydrophilic fixing phase thin layer
It is not less than 2cm with the outer ledge of described hydrophobic fixing phase thin layer with the average distance of described boundary line.
Double fixing phase chromatographic sheets of the present invention are further characterized by：Hydrophilic fixing phase thin layer and hydrophobic fixing phase
The thickness of thin layer is 100～200 μm.
Double fixing phase chromatographic sheets of the present invention are further characterized by：Angle is 10 °.
Double fixing phase chromatographic sheets of the present invention are further characterized by：Hydrophilic fixing phase thin layer and hydrophobic fixing phase
The thickness of thin layer is 100～200 μm, and angle is 10 °.
As a second aspect of the present invention, prepare above-mentioned double fixing phase chromatographic sheets it is characterised in that including following
Step：
Step one：Prepare hydrophilic polymeric liquid and hydrophobic polymeric liquid
First monomer, the first cross-linking agent, the first porogen and the first initiator are mixed to get hydrophilic polymeric liquid, first is single
Body is glycidyl methacrylate, and the first cross-linking agent is ethylene glycol dimethacrylate, and the first porogen is Hexalin,
First initiator is 2- hydroxy-2-methyl propiophenone, glycidyl methacrylate：Ethylene glycol dimethacrylate：Ring
The mass ratio of hexanol is 0.24：0.16：0.60,2- hydroxy-2-methyl propiophenone and glycidyl methacrylate and second two
Alcohol dimethylacrylate mixture quality is than for 0.01:1, second comonomer, the second cross-linking agent, the second porogen and second are drawn
Send out agent and be mixed to get hydrophobic polymeric liquid, second comonomer is butyl methacrylate, the second cross-linking agent is ethylene glycol dimethyl propylene
Acid esters, the second porogen is Hexalin and 1-4 butanediol, and the second initiator is benzoin methyl ether, butyl methacrylate：Second two
Alcohol dimethylacrylate：Hexalin：1-4 butanediol mass ratio is 0.24：0.16：0.41：0.19, benzoin methyl ether and methyl
Butyl acrylate and ethylene glycol dimethacrylate mixture quality are than for 0.01:1；
Step 2：Prepare hydrophilic fixing phase thin layer
Both sides between two pieces of glass plates are encased inside filter paper bar first, and two pieces of glass plates of clamping make mould, and mould is with straight
Its one end is immersed hydrophilic polymeric liquid by cube formula, and hydrophilic polymeric liquid fills the inner space of mould under capillary action, then will
Mould is placed at the 1cm～1.5cm under uviol lamp, irradiates 25min～35min, the wavelength of ultraviolet light is 254nm, promotes hydrophilic
Polymer fluid carries out polyreaction in mould, forms hydrophilic fixing phase thin layer between two pieces of glass plates；
Step 3：Prepare hydrophobic fixing phase thin layer
Remove mould, the glass plate of the side of taking off is as substrate, and marks boundary line on substrate, strikes off substrate upper border line
The hydrophilic fixing phase thin layer of side, and the both sides by substrate and boundary line are encased inside filter paper bar, and another piece of glass plate is covered
On substrate, mould made by clamping glass plate and substrate, and the blank end toward mould is slowly injected into hydrophobic polymeric liquid, and hydrophobic polymeric liquid exists
Fill the inner space of mould under capillarity, then by mould be placed in 1cm～1.5cm under uviol lamp at irradiation 25min～
35min, the wavelength of ultraviolet light is 254nm, promotes hydrophobic polymeric liquid to carry out polyreaction in mould, glass plate and substrate it
Between form hydrophobic fixing phase thin layer, meanwhile, hydrophobic fixing phase thin layer is bonded at boundary line with hydrophilic fixing phase thin layer and is connected, two
Person forms a double fixing phase thin layer, is attached on substrate；
Step 4：Activation processing
Remove described mould, the described substrate depending on described pair of fixing phase thin layer is immersed and in methanol or ethanol, processes 6
～12h, takes out, and after being dried, immersion concentration is the H of 0.3～0.6mol/L2SO4In solution, water bath processing 2 at 50～80 DEG C～
3h, takes out, and rinses, and after being dried, obtains described pair of fixing phase chromatographic sheet.
The preparation method of double fixing phase chromatographic sheets of the present invention is further characterized by：Two blocks of glass in step 2
Plate is before use through silanization pretreatment.
The preparation method of double fixing phase chromatographic sheets of the present invention is further characterized by：Step 2 and step 3
In, uviol lamp is double, and the power of the uviol lamp often arranged is 8w.
The preparation method of double fixing phase chromatographic sheets of the present invention is further characterized by：Two blocks of glass in step 2
Before use in silanization pretreatment, step 2 and step 3, uviol lamp is double to piece, and the power of the uviol lamp often arranged is
8w.
Invention effect and effect
The preparation method of the double fixing phase chromatographic sheets according to the present invention, due to preparing hydrophilic fixing phase on substrate
Mark boundary line after thin layer, and strike off the hydrophilic fixing phase thin layer of boundary line side, then prepare hydrophobic fixing phase at the place of striking off
Thin layer, and hydrophobic fixing phase thin layer at boundary line with hydrophilic fixing phase thin layer bonding be connected so that both are attached to side respectively
On the substrate of boundary line both sides, the double fixing phase thin layer of composition, thus obtain double fixing phase chromatographic sheets；And due to the present invention's
Hydrophilic fixing phase thin layer and hydrophobic fixing phase thin layer are manufactured separately in boundary line both sides, will not interfere with each other the control in both apertures
System, can obtain more preferably aperture such that it is able to improve the separating effect of chromatographic sheet.
According to double fixing phase chromatographic sheets of the present invention, because hydrophilic fixing phase thin layer and hydrophobic fixing phase thin layer are single
Solely prepare, therefore the uniform pore diameter of double fixing phase thin layers of formation and controlled, rather than as in prior art, original
The in the hole portion of thin layer connects side chain, and the therefore present invention can obtain more preferably pore-size distribution so that the uniform diameter in hole is distributed,
And ratio that the hole that is in mesopore range of diameter accounts for is maximum, thus improve chromatographic isolation effect.
Brief description
Fig. 1 is double fixing phase chromatographic sheets structural representation in an embodiment of the present invention；And
Fig. 2 is the effect diagram for chromatographic isolation for double fixing phase chromatographic sheets of the present invention.
Specific embodiment
Below in conjunction with being embodied as case, technical scheme is described further.
Fig. 1 is double fixing phase chromatographic sheets structural representation in an embodiment of the present invention.
As shown in figure 1, double fixing phase chromatographic sheets 10 include substrate and the double fixing phase thin layers being formed on substrate.
Substrate be rectangle glass plate, specifically length be 7cm, width be 2.6cm microscope slide.The center score of substrate
There is the boundary line 3 intersected with upper and lower sides sideline, the angle in boundary line 3 opposed vertical direction is 10 °.Double fixing phase thin layers are porous
Structure, be attached on substrate.The thickness of double fixing phase thin layers is 100 μm.Certainly the double fixing phase thin layers in the present embodiment
Thickness can also be other numerical value in 100～200 μm.
Double fixing phase thin layers include the hydrophilic fixing phase thin layer 1 with hydrophilic chromatographic function and have hydrophobic chromatography function
Hydrophobic fixing phase thin layer 2.The composition of hydrophilic fixing phase thin layer 1 is poly- (glycidyl methacrylate-ethylene glycol dimethyl third
Olefin(e) acid ester) integral material.The composition of hydrophobic fixing phase thin layer 2 is poly- (butyl methacrylate-ethyleneglycol dimethacrylate
Ester) integral material.
As shown in figure 1, hydrophilic fixing phase thin layer 1 is located at the left side of substrate, hydrophobic fixing phase thin layer 2 is located at the right side of substrate
Side.Hydrophilic fixing phase thin layer 1 and hydrophobic fixing phase thin layer 2 are porous, are attached to respectively on the substrate of boundary line 3 both sides on side
At boundary line 3, bonding connects,
In the present embodiment, the uniform pore diameter distribution of hydrophilic fixing phase thin layer 1 and hydrophobic fixing phase thin layer 2, and diameter
The ratio that the hole being distributed in mesopore range accounts for is maximum, is optimal pore-size distribution, double fixing phases of therefore the present embodiment are thin
Layer chromatography plate separating effect is very good.
Fig. 2 is the effect diagram for chromatographic isolation for double fixing phase chromatographic sheets of the present invention.
Fixing phase chromatographic sheets 10 double in Fig. 1 are used for separating 4 kinds of dyestuffs.From border in hydrophobic fixing phase thin layer 2
The mixed liquor of 4 kinds of dyestuffs is selected, apart from the top edge 0.5cm of hydrophobic fixing phase thin layer 2 at point sample at line 1cm.In figure is vertically empty
Line is the first dimension detaching direction, and arrow points to developing solvent flow direction.Horizontal dotted line is pointed to for the second dimension detaching direction, arrow
Agent flow direction.
Mixed liquor is completely dried after the first dimension is launched, and obtains the result as shown in Fig. 2 (a).It can be seen that after separating
There are three speckles.Hydrophobic fixing phase thin layer 2 has hydrophobic chromatography function, the therefore less C.I. 13020. of polarity and P-aminoazobenzene
Hydrophobic fixing phase thin layer 2 is separated, respectively in two speckles formed below of hydrophobic fixing phase thin layer 2.And polarity is larger
R6G do not separated with malachite green oxalate, formed mixed dot.
Then by mixed dot to two-dimensional development.Speckle in order to avoid separator well is destroyed, and to be opened up using filter paper bar
Open, by one section of immersion developing solvent of filter paper bar, the other end is attached to the edge of mixed dot, is sent to hydrophilic fixing phase thin layer
In 1, and the result obtaining as shown in Fig. 2 (b) after launching to separate.Hydrophilic fixing phase thin layer 1 has hydrophilic chromatographic function, therefore pole
Property larger R6G separated in hydrophilic fixing phase thin layer 1 with malachite green oxalate, form two speckles.
From figure 2 it can be seen that using the double fixing phase chromatographic sheets in the present embodiment, can will be complete for 4 kinds of dyestuffs
Separate, separating effect very well, illustrates that the double fixing phase chromatographic sheets in the present embodiment have hydrophilic chromatographic function simultaneously and dredge
Water chromatographic function, and separating effect is fine.
Wherein, boundary line 3 is arranged to 10 °, has certain inclination angle, is in order that mixed dot is nearer apart from border, more holds
Easily it is extended in hydrophilic fixing phase thin layer 1, not interfering with should speckle through separate C.I. 13020. and P-aminoazobenzene.Certainly
The inclination angle of the boundary line 3 of the present embodiment can also being actually needed according to material to be separated, be arranged to the random angle in 0 °～20 °
Degree.
The outer ledge of hydrophilic fixing phase thin layer 1 and hydrophobic fixing phase thin layer 2 and the average distance at least 2cm of boundary line 3,
It is to ensure that developing solvent can have enough flowing spaces so that molten in hydrophilic fixing phase thin layer 1 and hydrophobic fixing phase thin layer 2
Xie Yu material to be separated therein mass-energy is separately.If the distance of Edge Distance boundary line 3 is too small, can lead to launch insufficient, thing
Matter can not be effectively separated.
The preparation method of the double fixing phase chromatographic sheets employed in the present embodiment, can prepare above-mentioned double fixations
Phase chromatographic sheet 10, comprises the following steps：
(1) silanization treatment substrate
Take two pieces of microscope slides as shown in fig. 1, after using water and alcohol flushing successively, in the NaOH solution of immersion 0.5mol/L
30min, makes slide surface modify upper hydroxyl；Wash with water after taking-up, then immerse 30min in the HCl/water solution of 0.5mol/L, make
Hydroxyl fully exposes；Microscope slide is dried at 60 DEG C 1h, after cooling, immerses 3- (isobutene. acyl-oxygen) propyl group three of 20% (v/v)
In the ethanol solution of methyl-monosilane overnight, make microscope slide alkylation；It is placed in dehydration 1.5h at 35 DEG C after taking-up, finally will handle well
Microscope slide be placed in dark place preserve.
(2) hydrophilic polymeric liquid and hydrophobic polymeric liquid are prepared
Choose glycidyl methacrylate as the first monomer, weigh 1.92g；Choose ethyleneglycol dimethacrylate
Ester, as the first cross-linking agent, weighs 1.28g；Choose Hexalin as the first porogen, weigh 4.8g；Choose 2- hydroxyl -2- first
Base propiophenone, as the first initiator, weighs 0.032g；After mentioned reagent is mixed, ultrasonic 15min makes it be sufficiently mixed and removes
Gas, obtains hydrophilic polymeric liquid.
Choose butyl methacrylate to make second is monomer, weighs 1.92g；Choose ethylene glycol dimethacrylate conduct
Second cross-linking agent, weighs 1.28g；Choose Hexalin and 1-4 butanediol as the second porogen, weigh Hexalin 4.8g, weigh
1-4 butanediol 1.52g；Choose benzoin methyl ether as the second initiator, weigh 0.032g；After mentioned reagent is mixed, ultrasonic
15min makes it be sufficiently mixed and degasification, obtains hydrophobic polymeric liquid.
(3) prepare hydrophilic fixing phase thin layer
It is encased inside two filter paper bars in the middle of the microscope slide after two pieces of activation, two filter paper bars are distributed in the both sides of microscope slide,
Make simple mould with clamp.Its one end is immersed hydrophilic polymeric liquid with standing manner by mould, and hydrophilic polymeric liquid is in hair
Spy, with the lower inner space that can fill mould, infiltrates the other end of microscope slide.
In fume hood, mould is placed in irradiation 30min under double uviol lamp, uviol lamp lies in a horizontal plane in above mould
At 1.2cm, the power of uviol lamp is 8w, and wavelength is 254nm.Hydrophilic polymeric liquid carries out polyreaction on microscope slide, generates poly-
(glycidyl methacrylate-ethylene glycol dimethacrylate) integral material, thus form hydrophilic fixing phase thin layer 1.
Carry out polyreaction in fume hood, good radiating can be reached, eliminate the impact to polymerization for the temperature.Now, hydrophilic solid
The side chain determining phase thin layer 1 is hydrophobic epoxy radicals, and therefore, hydrophilic fixing phase thin layer 1 now shows hydrophobicity.
(4) prepare hydrophobic fixing phase thin layer
Remove mould, the microscope slide of the side of taking off, as substrate, and thereon by marking boundary line 3 shown in Fig. 1.Then,
Strike off hydrophilic fixing phase thin layer 1 with pocket knife in boundary line 3 side, and be again encased inside two filter paper bars in the region struck off.Refitting
Mould, is slowly injected into hydrophobic polymeric liquid with syringe toward the blank end being stripped off hydrophilic fixing phase thin layer 1 so that hydrophobic polymeric liquid
Stripping areas in filling mould.New filter paper bar needs by the both sides of substrate and boundary line 3, prevents hydrophobic polymeric liquid from permeating
Centre to hydrophilic fixing phase thin layer 1.
In fume hood, mould is placed in irradiation 30min under double uviol lamp, uviol lamp lies in a horizontal plane in above mould
At 1.2cm, the power of uviol lamp is 8w, and wavelength is 254nm.Hydrophobic polymeric liquid carries out polyreaction on substrate, generates poly- (first
Base butyl acrylate-ethylene glycol dimethacrylate) integral material, thus forming hydrophobic fixing phase thin layer 2.Now, hydrophobic
The side chain of fixing phase thin layer 2 is hydrophobic butyl, and therefore hydrophobic fixing phase thin layer 2 is hydrophobicity, has hydrophobic chromatography function.
Meanwhile, hydrophobic polymeric liquid is bonded at boundary line 3 with the edge of hydrophilic fixing phase thin layer 1, will be thin for hydrophilic fixing phase
Layer 1 and hydrophobic fixing phase thin layer 2 link together.This is because hydrophilic polymeric liquid carries out polyreaction, and to form hydrophilic fixing phase thin
After layer 1, also remain a part of hydrophilic polymeric liquid in hydrophilic fixing phase thin layer 1, some first monomers are not complete with the first cross-linking agent
Full polymerization, and the group also coming out, so hydrophobic polymeric liquid still can be formed altogether with the edge of hydrophilic fixing phase thin layer 1
Valence link, thus be bonded together.And because hydrophobic polymeric liquid is slowly injected in mould, the hydrophobic polymeric liquid of therefore injection is not
Can penetrate in the middle of the hydrophilic fixing phase thin layer 1 being polymerized, the simply EDGE CONTACT of hydrophilic fixing phase thin layer 1.
Therefore, hydrophilic fixing phase thin layer 1 and hydrophobic fixing phase thin layer 2 are bonded connection at boundary line 3, and both form one
Double fixing phase thin layers, are attached on substrate.
(5) activation processing
Remove mould again, attached lamellate substrate is immersed in ethanol and processes 12h, get rid of hydrophilic fixing phase thin layer 1
With the porogen in hydrophobic fixing phase thin layer 2, and unreacted monomer and cross-linking agent.By attached lamellate substrate from ethanol
Take out, be dried at room temperature for.
The H of immersion 0.5mol/L2SO4In aqueous solution, 60 DEG C of water bath processing 3h.Before sulfuric acid treatment, hydrophilic fixing phase is thin
The side chain of layer 1 is hydrophobicity epoxy radicals, shows hydrophobicity, but sulfuric acid treatment can make epoxy ring-opening form o-dihydroxy,
Hydrophilic greatly enhances, so that hydrophilic fixing phase thin layer 1 shows hydrophilic, thus possessing the function of hydrophilic chromatographic.This
When, double fixing phase thin layers have hydrophilic chromatographic function and hydrophobic chromatography function simultaneously.
Then will take out with the substrate of double fixing phase thin layers, with substantial amounts of water with ethanol rinse to neutral, be placed in 40
DEG C drying；Thus obtaining double fixing phase chromatographic sheets 10, this pair of fixing phase chromatographic sheet has hydrophobic chromatography and hydrophilic color
Two kinds of functions of spectrum.
Embodiment effect and effect
The preparation method of the double fixing phase chromatographic sheets according to the present embodiment, due to preparing hydrophilic fixation on substrate
Mark boundary line after phase thin layer, and strike off the hydrophilic fixing phase thin layer of boundary line side, then prepare hydrophobic fixation at the place of striking off
Phase thin layer, and hydrophobic fixing phase thin layer at boundary line with hydrophilic fixing phase thin layer bonding be connected so that both are attached to respectively
On the substrate of boundary line both sides, the double fixing phase thin layer of composition, thus obtain double fixing phase chromatographic sheets；And due to the present invention
Hydrophilic fixing phase thin layer and hydrophobic fixing phase thin layer be manufactured separately in boundary line both sides, the control in both apertures will not be interfered with each other
System, can obtain more preferably aperture such that it is able to improve the separating effect of chromatographic sheet.
According to double fixing phase chromatographic sheets of the present invention, because hydrophilic fixing phase thin layer and hydrophobic fixing phase thin layer are single
Solely prepare, therefore the uniform pore diameter of double fixing phase thin layers of formation and controlled, rather than as in prior art, original
The in the hole portion of thin layer connects side chain, and the therefore present invention can obtain more preferably pore-size distribution so that the uniform diameter in hole is distributed,
And ratio that the hole that is in mesopore range of diameter accounts for is maximum, thus improve chromatographic isolation effect.
Certainly technical scheme is not limited in the description in above example.Irradiation time under uviol lamp is also
Arbitrarily can select in 25min～35min.The H that can also immerse with the substrate of double fixing phase thin layers2SO4Aqueous solution dense
Degree arbitrarily can also select in 0.3～0.6mol/L, and the temperature of water bath processing arbitrarily can also select in 50～80 DEG C, water
The time that bath is processed arbitrarily can also select in 2～3h.Place in methanol can also be immersed with the substrate of double fixing phase thin layers
Reason, process time arbitrarily can also select in 6～12h.
Claims (4)
1. the preparation method of a kind of pair of fixing phase chromatographic sheet is it is characterised in that comprise the following steps：
Step one：Prepare hydrophilic polymeric liquid and hydrophobic polymeric liquid
First monomer, the first cross-linking agent, the first porogen and the first initiator are mixed to get described hydrophilic polymeric liquid, first is single
Body is glycidyl methacrylate, and the first cross-linking agent is ethylene glycol dimethacrylate, and the first porogen is Hexalin,
First initiator is 2- hydroxy-2-methyl propiophenone, glycidyl methacrylate：Ethylene glycol dimethacrylate：Ring
The mass ratio of hexanol is 0.24：0.16：0.60,2- hydroxy-2-methyl propiophenone and glycidyl methacrylate and second two
Alcohol dimethylacrylate mixture quality is than for 0.01:1, second comonomer, the second cross-linking agent, the second porogen and second are drawn
Send out agent and be mixed to get described hydrophobic polymeric liquid, second comonomer is butyl methacrylate, the second cross-linking agent is ethylene glycol dimethyl
Acrylate, the second porogen is Hexalin and 1-4 butanediol, and the second initiator is benzoin methyl ether, butyl methacrylate：
Ethylene glycol dimethacrylate：Hexalin：1-4 butanediol mass ratio is 0.24：0.16：0.41：0.19, benzoin methyl ether with
Butyl methacrylate and ethylene glycol dimethacrylate mixture quality are than for 0.01:1；
Step 2：Prepare hydrophilic fixing phase thin layer
Both sides between two pieces of glass plates are encased inside filter paper bar first, and two pieces of glass plates of clamping make mould, and described mould is with straight
Its one end is immersed described hydrophilic polymeric liquid by cube formula, and described hydrophilic polymeric liquid fills the inside of described mould under capillary action
Space, then described mould is placed at the 1cm～1.5cm under uviol lamp, irradiates 25min～35min, and the wavelength of ultraviolet light is
254nm, promotes described hydrophilic polymeric liquid to carry out polyreaction in described mould, is formed described between described two pieces of glass plates
Hydrophilic fixing phase thin layer；
Step 3：Prepare hydrophobic fixing phase thin layer
Remove described mould, the described glass plate of the side of taking off is as substrate, and marks boundary line on the substrate, strike off described
The hydrophilic fixing phase thin layer of described boundary line side on substrate, and the both sides by described substrate and described boundary line are encased inside filter paper
Bar, another piece of glass plate is covered on the substrate, clamps described glass plate and mould made by described substrate, toward described mould
Blank end be slowly injected into described hydrophobic polymeric liquid, described hydrophobic polymeric liquid fills the inner space of described mould, then by institute
State mould and be placed in irradiation 25min～35min at 1cm～1.5cm under uviol lamp, the wavelength of ultraviolet light is 254nm, promotes described dredging
Water polymer fluid carries out polyreaction in described mould, forms described hydrophobic fixing phase between described glass plate and described substrate
Thin layer, meanwhile, described hydrophobic fixing phase thin layer is bonded at described boundary line with described hydrophilic fixing phase thin layer and is connected, both groups
Become a double fixing phase thin layer, depend on the substrate；
Step 4：Activation processing
Remove described mould, by depend on process 6 in the described substrate immersion methanol of described pair of fixing phase thin layer or ethanol～
12h, takes out, and after being dried, immersion concentration is the H of 0.3～0.6mol/L2SO4In solution, water bath processing 2～3h at 50～80 DEG C,
Take out, rinse, after being dried, obtain described pair of fixing phase chromatographic sheet.
2. the preparation method of according to claim 1 pair of fixing phase chromatographic sheet is it is characterised in that in described step 2
Two pieces of glass plates are before use through silanization pretreatment.
3. according to claim 1 pair of fixing phase chromatographic sheet preparation method it is characterised in that described step 2 and
In step 3, described uviol lamp is double, and the power of the described uviol lamp often arranged is 8w.
4. the preparation method of according to claim 1 pair of fixing phase chromatographic sheet is it is characterised in that in described step 2
Before use through silanization pretreatment, in described step 2 and step 3, described uviol lamp is double to two blocks of sheet glass, often arranges
Described uviol lamp power be 8w.
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| US20190170713A1 (en) * | 2016-12-26 | 2019-06-06 | Panasonic Intellectual Property Management Co., Ltd. | Thin layer chromatography plate and sample analysis method using same |
| CN112748212B (en) * | 2019-10-31 | 2024-06-07 | 中国石油化工股份有限公司 | Chromatographic rod preparation container and chromatographic rod preparation method |
| CN115166127A (en) * | 2022-07-26 | 2022-10-11 | 吉首大学 | Thin layer identification method from complex two-dimensional to simple one-dimensional |
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|---|---|---|---|---|
| US4313906A (en) * | 1979-08-17 | 1982-02-02 | Whatman, Inc. | Two dimensional two phase thin layer chromatography plate and method |
| US7473367B2 (en) * | 2002-06-26 | 2009-01-06 | Dionex Corporation | Monolithic column |
| US9217734B2 (en) * | 2009-07-01 | 2015-12-22 | Brigham Young University | Thin layer chromatography plates and related methods |
| JP5941405B2 (en) * | 2010-05-27 | 2016-06-29 | 株式会社ダイセル | Method for detecting sample by thin layer chromatography, thin layer chromatography plate, and method for producing the same |
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