CN85105260A - The parting material of thin-layered chromatography - Google Patents
The parting material of thin-layered chromatography Download PDFInfo
- Publication number
- CN85105260A CN85105260A CN 85105260 CN85105260A CN85105260A CN 85105260 A CN85105260 A CN 85105260A CN 85105260 CN85105260 CN 85105260 CN 85105260 A CN85105260 A CN 85105260A CN 85105260 A CN85105260 A CN 85105260A
- Authority
- CN
- China
- Prior art keywords
- silica gel
- acid
- mol
- parting material
- catalyst
- 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.)
- Pending
Links
Landscapes
- Catalysts (AREA)
Abstract
The present invention relates to a kind of a kind of new separation material of thin-layered chromatography that is coated with one deck adsorbent for the basis on carrier, it is formed by the layer of silica gel of silanizing agent surface modification after by coating.It is characterized in that a coverage fixing and that can regulate control is arranged, anti-phase material adjustable range be can be 0.15～0.8 μ mol/m
2With to water wetted material 1.2～2.5 μ mol/m
2The invention still further relates to the method for producing this parting material.
Description
The book layer chromatography is enlarging the analytical method of using because its rapidity is a kind of continuation, and owing to developing continuously and improving, its efficient is constantly improving.By HPTLC technology (high-performance book layer chromatography, High Performance Thin Layer ChromatograPhy) obtain at last further migrating result in the high pressure liquid chromatography (HPLC), but the HPTLC-analytical technology shows and will elect between the two in quick and price.And book layer chromatography/HPTLC development of technology is to build on Bio-sil, and it is used mainly as absorbent or carrier in the book layer chromatography.
The silica gel surface of particularly having adopted with the organic group chemical modification (for example sees that magazine introduces Journal High Resol, Chromatogr.Comm, 3; 214～240,1980) make range of application enlarge significantly, because the Si-OH base of silica gel nature polarity might transform by the chemical reaction with the organic molecule of suitable lipophilic or part lipophilic, promptly change into hydrophobic (anti-phase) or part hydrophobic grouping.
Another development of book layer chromatography technology is modification in position, i.e. chemical modification on a layer of silica gel that processes, for example, resemble and in DE-PS-2712113 or DE-PS-2809137, reported, can produce another kind like this as the even filling of one deck and structure aspect.
In the production method of known chemical modification silica gel, have organic group modified adsorbent topped degree mainly by can with the decision of the kind of the modifying agent of Si-OH radical reaction in the silica gel structure.In order to produce high as far as possible conversion degree, use has the halogen silane of substitution reaction ability accordingly as modifying agent usually.Press DE-PS-2426306, when silanization, use the alkoxy silane of reaction carriers, when having catalyst to exist simultaneously, can make the silica gel surface that one very high topped degree is arranged.Though high conversion degree has guaranteed to have between hydrophobic carrier matrix and the hydrophobic substance good interaction, such problem also can occur, hydrophobic modified silica-gel layer is because moisture in a large number flowing materials and reagent injected and no longer be wettable.
In order to guarantee desired water wettability, must reduce the hydrophobicity of the layer of silica gel of modification.Use very few halogen silane or before coating the mixing of minimum modification with unmodified silica gel, having seen in the practice attends the meeting brings important disadvantages.The alkoxyl or the aralkoxy silane that are reduced in application response carrier in the general reality of hydrophobicity of in-situ modified layer of silica gel carry out chemical modification, but the strong shortcoming that reduces of topped degree is often arranged.Original antiphase effect has not often been reached.
When layer of silica gel for example has epoxy radicals or amino alkyl chain and carries out chemical modification with the organic molecule that contains the polarity hydrophilic group, because corresponding halogen silane does not exist, generally can only use alkoxyl or aralkoxy silane, therefore to have be lower to such modified silica-gel in principle, and part is too low topped degree.In such method of modifying, higher surface concentration may be beneficial to, because the very high group of lead-in portion polarity, can bring desirable water wettability even the pure hydrophobically modified layer during with maximum conversion is in any case compared.
Therefore, being faced of task is to develop with the parting material of silica gel as the carrier basis for the book layer chromatography, it has low, uniform topped degree on the one hand after layer of silica gel is with (hydrophobic) anti-phase material modification, but topped degree like this makes the book layer can have the water wellability, realize by desirable degree for the anti-phase effect on the other hand, topped degree is again that sufficient Enough is high, so just can make quite hydrophobic material can carry out chromatographic isolation in moisture liquid phase systems.In order to use widely, require behind modified-reaction, can control the topped degree of the layer of silica gel that water can soak into.Also have a task in addition, develop hydrophilic modification book layer chromatography parting material, make controllable topped degree same after its modification apparently higher than material corresponding to DBP2713113 and DBP2809137 production.
Find that now general HPTLC-finished product sheet can cause apparently higher than undressed uniform topped degree with the catalyst solution preliminary treatment earlier before the modification in position at the alkoxyl or the aralkoxy silane of layer of silica gel with reaction carriers.In whole process, comprising that preliminary treatment can Shi Zai No be removed under the air humidity carries out.Be surprised to find that in addition by quantitatively and mainly being the composition that changes catalyst solution qualitatively, topped degree can be adjusted by different value by Enough first.This effect is not confined to pure (hydrophobic) anti-phase material, and can use water wetted material yet, just can reach controllable bigger surperficial topped degree at this moment.Because this finds, the parting material that provides the book layer chromatography that adapts to various separation problems ideally to use.In order to grasp the interactional influence of hydrophobic/hydrophilic, the accurate adjustment by hydrophobic on the layer of silica gel and water-wetted surface regional percentage makes it also can be applicable to moisture liquid phase substance system, can obtain excellent chromatographic isolation by Enough like this.
Xian You Ji Shu No has proposition to can be the technology solution that the book layer chromatography is opened up many new application possibilities.Mealy solid particle is being arranged and removing in the presence of the catalyst of moisture content though in DE-PS-2426306, reported, improve the method for modifying agent surface concentration by the silanization of oh group, but for the professional, both can not carry according to this invention, also can not get the technological guidance of this invention, particularly about controlling the guidance of topped degree.
An aspect of of the present present invention is about being new separation material base, that be used for the book layer chromatography being coated with one deck adsorbent on the carrier material and carrying out the carrier that the layer of silica gel of surface modification forms with silanizing agent after coating, it is characterized in that the wettable layer of silica gel surface of water has 0.15～0.8 μ mol/m in anti-phase (RP) material
2Or 1.2-2.5 μ mol/m arranged in water wetted material
2Even overcoat.Wherein being that the reverse material (RP18) of base has 0.3～0.5 μ mol/m at the C18-alkyl chain
2Even overcoat and to the C8-alkyl chain for the base reverse material (RP8) have 0.35～0.7 μ mol/m
2The corresponding parting material of overcoat and water wetted material had 1.5～2.3 μ mol/m
2Evenly a kind of parting material of overcoat is for well.
Another aspect of invention is about producing the method for this parting material.This method is: in modification, the wettable silica gel surface of water is soaked with catalyst solution earlier before handling with silanizing agent and it evenly is coated with.The Silanization reaction that catalyst energy catalysis silica gel is familiar with.Wherein a kind of desirable method is to be coated with and modification not getting rid of under the moisture content.A kind of in addition method preferably is that for control surface modification on request, catalyst solution is preferentially adjusted in 0.01～20 weight % concentration range and used.These methods are preferably used alkoxyl or aralkoxy silane as silanizing agent in order to produce parting material of the present invention in addition.Content of the present invention also comprises the method for the parting material of inventing as Catalyst Production with chloroacetic chloride and glacial acetic acid mixture, with use trichloroacetic acid, dichloroacetic acid or chlorine ester acetic acid or trifluoracetic acid, difluoro acetic acid or fluorine acetic acid are as the method for Catalyst Production parting material of the present invention.
Parting material of the present invention have by hydrophobic, hydrophilic or part hydrophobic/hydrophilic residue can produce can harmonize shown very big inhomogeneity overcoat by clearly defined.
The topped degree of anti-phase material (RP) changes at 0.15～0.8 μ mol/m
2, the C18 alkyl chain is preferably in 0.3～0.5 μ mol/m for basic anti-phase material
2, to the C8 alkyl chain be the base the anti-phase material preferentially at 0.35～0.7 μ mol/m
2, to water wetted material at 1.2～2.5 μ mol/m
2, preferentially at 1.5～2.3 μ mol/m
2Change.
This surface topped degree γ (μ mol/m
2) define (seeing colloid and interface Science 6(1976) 95～137 according to Ke Wanci (Kova'ts)).Parting material of the present invention also can indicate with their conversion degree.It represents that with % it is relevant with maximum accessible topped degree, and this topped degree is because the influence in space is limited in about 4 μ mol/m
2
To reverse material, topped degree can reach the topped degree according to the available any maximum of prior art, and the silica gel surface hydrophobic of modification reduces thus.Parting material of the present invention also has the water wettability in certain limit.To the hydrophilic modifying layer, its aliphatic or the aromatic yl aliphat chain by polar group, for example, epoxy or amino the replacement, can obtain topped degree and might adjust to the parting material that is higher than by the modified layer of DBP2712113 and DBP2809137 gained significantly.
Modified silica-gel layer of the present invention makes the range of application as book layer chromatography parting material obtain huge development.Parting material of the present invention in addition also has the identical advantage of modification parting material in position by DBP2712113 and DBP2809137, it shows as excellent repeatability, water content and air humidity insensitivity to layer, the high-purity of layer, fill uniformly and laminar surface structure and when production, in the product stage less problem is arranged especially.
The production method of HPTLC-parting material of the present invention is simple especially unexpectedly.Promptly, before transforming with silane originally, be coated with equably with catalyst solution finished product layer (contrast DE-PS-2426306).
As all suiting of all known Silanization reactions that can catalysis silica gel on the catalyst principle, from relevant document, can possibility widely be arranged for what the professional selected for use, inorganic and the organic acid of general application, and the derivative of their ability that responds and inorganic and organic base.Preferentially select the respond derivative of ability of inorganic and organic acid and they for use, the organic acid of replacement is optimum.
Adaptable inorganic acid can be considered HCl, HBr, HJ, HF, H as an example
2SO
4, HNO
3, H
3PO
4, H
3BO
3, HClO
4, HBrO
4, HJO
4The mixture that two or more components are perhaps arranged, particularly suitable is all hydrogen halides.Can consider the acid of carbon containing or acid, sulfonic acid or the amino acid of the carbon containing that replaces as organic acid, but the acid of carbon containing and its substitutive derivative are more suitable, the mixture of using various single components also is possible.The best example of the acid of the acid of adaptable carbon containing or the carbon containing that replaces can list: formic acid, acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, chloroacetic acid, dichloroacetic acid, trichloroacetic acid or fluorine acetic acid, difluoro acetic acid and trifluoracetic acid.Acetic acid and fluoridize and the acetic acid of chlorination suitable especially.
As the particularly suitable halide that acid is arranged of the acid derivative of the outstanding carbon containing of the ability of responding, outstanding especially have chloride and a bromide, as chloroacetic chloride or acetyl bromide, corresponding acid anhydride arranged in addition, azide or ester.
A kind of in addition acid of and multiple carbon containing and (or) mixture of the acid derivative, particularly haloid acid of one or more abilities that respond is more suitable.Can be called having of antigravity system separately:
Chloroacetic chloride/acetic acid, chloroacetic chloride/propionic acid, propionyl chloride/acetic acid,
Propionyl chloride/propionic acid, chloroacetic chloride/formic acid, chloroacetic chloride/butyric acid,
Butyl chloride/acetic acid, butyl chloride/propionic acid, butyl chloride/formic acid,
Chloroacetic chloride/valeric acid, valeric chloride/valeric acid, propionyl chloride/butyric acid,
Propionyl chloride/valeric acid, formyl chloride/formic acid, formyl chloride/acetic acid,
Chloroacetic chloride/acetic acid/propionic acid, chloroacetic chloride/acetic acid/formic acid,
Chloroacetic chloride/propionyl chloride/acetic acid, chloroacetic chloride/propionyl chloride/propionic acid and chloroacetic chloride/propionyl chloride/formic acid.
Acid in the mixture of enumerating also can be used corresponding replacement acid substitution, and the suitable fluorine or chlorine that has replaces acid, difluoro or dichloro replacement acid or trifluoro or trichlorine replacement acid.The catalyst mixture that chloroacetic chloride and acetic acid are formed is more suitable.
As inorganic base at first is ammonia.As organic base can demonstrate for example as pyridine, two and triethyl-amine, butylamine or ethylenediamine.
Catalyst can concentrate, in case of necessity also can gaseous state or steam, or solution, particularly weak solution state exist.At first consider organically with the organic solvent of the solvent, particularly polarity that can mix, methyl alcohol, ethanol, normal propyl alcohol, isopropyl alcohol, n-butanol, methyl-propyl alcohol are arranged in case of necessity as alcohols with water as solvent.But also acetone, methyl ethyl ketone or small amount of polar solvent such as diox, carrene, dichloroethanes and trichloroethanes.Be at last non-polar solven such as benzene, nitro benzene,toluene,xylene, n-hexane or normal heptane, its prerequisite be catalyst or catalytic component in corresponding solvent, have sufficient Enough solubility or with their good mixing.Solvent can be dry, also can add certain water gaging.
The concentration of catalyst or catalyst mixture changes between 0.01%～20 weight % in soaking solution, in the solvent.Best concentration is 0.05～10%.Preferential low concentration, the preferential high concentration of selecting in weak acid or weak base selected in strong acid or highly basic.In catalyst mixture, single component relative scale changes in the scope of broad.At two components, ratio was with 1: 9～9: 1 in the system, and particularly 1: 9,2: 8,3: 7,4: 6,5: 5,6: 4,7: 3,8: 2 and 9: 1 are for well.
Be coated with the time between 1～20 minute with catalyst solution, preferably 8～12 minutes.The silica gel sheet is preferentially applied in 0.8～1.0 liter of catalyst solution, has through adjusting the change degree No that water content provides in modification the time on the surperficial activated silica gel sheet of modification influential at No.Do not require and carry out the predrying of plate or activation.More do not need deaeration moisture with the DE-PS2426306 method.In order to remove unnecessary catalyst, after plate is with the catalyst solution pre-coating or directly modification or be more preferably cleaning process through one or many.And this is impossible according to method that DE-PS2426306 reported, and cleaning process is used cited solvent usually, each clean and the solvent volume of every block of plate is upgraded to 0.7～1.0, and clean plate is placed on and is preferably 8～12 minutes in the cleaning solution at every turn.
Undertaken by known method (for example DE-OS-1712113) for the layer of silica gel chemical modification behind the painting catalyst, modification is that layer of silica gel is flooded or immersion with silanizing agent.For example raw material can be immersed in the silanizing agent solution or this solution of jetting, using for applied silanizing agent is that the common solvent of inertia is as solvent.But the priority application boiling point is 30 ℃～180 ℃ a organic solvent, the hydrocarbon of chloro for example, as carrene and chloroform and (or) dichloroethanes and trichloroethanes or fragrance or aliphatic hydrocarbon.
The alkoxyl of application response carrier or aralkoxy silane (R-SiX
3Type) as silanizing agent.Wherein R represents a unsubstituted alkyl group or aralkyl group when the modification of (hydrophobic) anti-phase, when hydrophilic modifying, represent to have the substituted alkyl or the aralkyl of polar group, X represents alkoxyl, aralkoxy or alkyl must at least one X be alkoxyl or aralkoxy in the per molecule wherein.
R can be the alkyl chain of the branch of 1～20 carbon atom where necessary, and alkyl chain is 8 or 18 carbon atoms preferably.
If R under the hydrophilic modifying situation, replaces with polar group, can consider as substituting group, as hydroxyl, amino, epoxy radicals, cyano group, halogen, ammonium, sulfonium or carboxyl, preferentially be epoxy radicals or amino as substituting group.A large amount of silanization materials can know from document also all and can produce with known similarity method that method of the present invention is suitable for the modification of known adsorbent surface equally.Depend mainly on layer of silica gel thickness and with the silica gel specific surface of making coatings as the consumption of the silanizing agent of surface modification.For the silanol base that contacts that makes untreated silica gel obtain topped completely, the silanizing agent that every square metre silica gel must minimum placement 10 μ mol, prerequisite is to use excessive silanizing agent, for example 0.1～1mmol/m
2In some cases, bigger excessive having many good qualities after soaking into silanizing agent, then dripped parting material only, carries out embathing repeatedly subsequently, to remove excessive silanization material and to clean modified layer.Desired cleaning process is mainly by the method for reporting in patent documentation 2712113 and 2809137.
All general parting materials that have the thin layer chromatography (tlc) layer of silica gel on carrier all can be used as raw material and use, for example resemble report among the DOS2524065 high efficiency parting material also like this.All general materials all can be used as carrier, wherein at first are glass plates.Paper tinsel also can use, and for example aluminium foil or plastic foil, the majority that can smear are that suspension is applied to common applicator or coating apparatus and obtains layer of silica gel on the carrier material.In suspension, also to add the binding agent that improves adherence and wearability, add indicator when needing.As the only organic bond that is to use Deutsche Bundespatent communique 1442446 or enumerates in DAS1517929 of adhesive, the indicator of frequent application is a fluorescence indicator.The magnesium tungstate that absorbs at ultraviolet light 254nm place is optimum, and (DBP2816574) the general consumption of adhesive is that 0.1～about 10% indicator consumption is 0.5～5 weight %.The layer of silica gel thickness of parting material of the present invention, as at present common book layer chromatography parting material, common thickness is 100～300 μ m exceptions or because different special purposes, parting material also can produce than book or thicker separating layers of material.The specific surface of silica gel is 1～1000m
2/ g, most applications is 200～800m
2/ g.
The water wettability of modified silica-gel layer depends on phase separately among the present invention.RP-18-material (the unsubstituted straight chained alkyl that 18 carbon atoms are arranged) is 0.55 μ mol/m at topped degree generally
2The time also have the water wettability.RP-8-material (8 unsubstituted straight chained alkyls of carbon atom are arranged).Its topped degree is about 0.7 μ mol/m
2The time also have the water wettability.
Control parameter to corresponding adjustable release agent among the present invention mainly is the composition of catalyst solution or mixed catalyst.The professional can select coating according to desired end product, or by prepare optimal solution by empirical experiment.Accessible topped degree of table 1 expression modification parting material of the present invention and the relation of in different modified silica-gel layers, producing the catalyst/solvent of exemplary use.In order relatively to have provided respective value by DBP2712113 and the 2809137 HPTLC parting materials of producing.The condition of being given is for the demonstration ， No that understands work any restriction to be arranged purely.Relevant embodiment provides as recommendation.
Can see that from table 1 this parting material can obtain not only that lower (RP-18, RP-8) topped degree also can obtain high topped degree (DIOL) and it should be noted that especially DIOL-modification parting material has very high topped degree compared with the prior art.
Table 2 is illustrated in that the desired solvent of catalyst still can exert an influence to topped degree under the identical condition.Given solvent it must be understood that to being exemplary purely.
Table 3 has provided the topped degree or the conversion degree of parting material.When producing them, when other conditions are identical, use different catalyst and come modification (example 2).The concentration of selection of catalysts and they also it must be understood that to being pure exemplary.Just as noted in Table 3, catalyst type has significant feature to the topped degree of parting material of the present invention.Topped degree can be done corresponding adjusting, and is the same as what show well in the embodiment of chlorination and the acetic acid of fluoridizing.
The special antigravity system of unexpectedly being made up of two or more catalyst components has amazing big variation on the controllability of topped degree, this in what ratio puts into each other in each component and decides.Proposed to table 4 property enumerated all can be separately as chloroacetic chloride and the ratio between the glacial acetic acid of catalyst and relation between the carbon content of RP-18HPTLC-parting material of direct relation is arranged with topped degree.Compare with the effect of single component, this antigravity system is often showing synergy aspect the topped degree.
The variable situation of topped degree and activated silica gel surface hydrophobic make considerable hydrophobic-hydrophilic substance and compounding substances be separated into possibility with the book layer chromatography, therefore special parting material be provided.Owing to use moisture solvent system, enlarged range of application greatly.Therefore also provided separation means thin tuning in addition.Because parting material of the present invention makes the range of application of book layer chromatography obtain conclusive expansion.
Embodiment
Below cited embodiment only distinguish over kind and the composition and the employed silane kind of applied catalyst.
All use 60F254S in all cases, 10 * 20Cm, HPTLC-silica gel finished product sheet, it is by E, Mike (E.Merck), Da Musidate (DarmStadt) produces.The product glass separator box of De Shajia (DcSaga) factory is as the inundator of all production stages.
The general production stage that is suitable for is as follows:
1) makes painting catalyst or mixed catalyst on the plate in the corresponding solution by being immersed in.
2) plate is immersed in the corresponding organic solvent, to remove unnecessary catalyst.
3) plate is immersed in makes its modification in the corresponding solution of silane.
4) plate is immersed in the mixed solvent of corresponding solvent and (perhaps) opposed polarity repeatedly continuous wash.
Embodiment 1:
But produce the good HPTLC-layer RP-18 of water wellability
To 1) be dissolved in the 900ml methyl alcohol with the dense HCl of 0.9ml that (=0.04%HCl) solution soaks the HPTLC finished silicon film of 60F254S 10 minutes.
To 2): the centre of carrying out 10 minutes at 900ml methyl alcohol with in 900ml toluene is cleaned.
To 3): in containing the toluene solution of 10% methyl octadecyl dimethoxy silane, 900ml places 20 minutes so that its silanization.
To 4): plate is placed on for 2 times is 900ml toluene, 900ml methylene chloride (1/1) is placed on for 2 times and is in 900ml acetone (1/1) and the 900ml methyl alcohol each 10 minutes and cleans
Embodiment 2:
The production of the HPTLC-production board RP-18 that lucky water is wettable.
To 1): HPTLC plate KG60 is placed on the immersion coating that the solution of being formed in the 900ml toluene (ratio 7: 3,10% total concentration) carried out 10 minutes with one by 63ml chloroacetic chloride and 27ml ice vinegar.
To 2): clean with the centre that 900ml toluene carried out 10 minutes.
To 3): similar embodiment 1.
To 4): similar embodiment 1.
Embodiment 3:
The production of the HPTLC-production board RP-18 that water is can be fine wetting.
To 1) HPTLC plate KG60 is placed on the immersion coating that the solution of being formed in the 900ml toluene (ratio 9: 1,10% total concentration) carried out 10 minutes with one by 81ml chloroacetic chloride and 9ml glacial acetic acid.
To 2), 3) and 4): similar embodiment 2.
Embodiment 4:
The production of the HPTLC production board RP-18 that lucky water is wettable.
To 1), 2): similar embodiment 2.
To 3): use methyl octadecyl dimethoxy silane, similar embodiment 2 in addition.
To 4) similar embodiment 2.
Embodiment 5:
The production of HPTLC processing plate Di Aoer (Diol).
To 1): by 4, the 5ml trichloroacetic acid soaks coating 10 minutes to HPTLC plate KG60 in the solution that 900ml toluene (0.5% total concentration) is formed a kind of.
To 2): clean in the middle of the cancellation.
To 3): contain the γ-toluene solution of glycidyl oxygen propyl trimethoxy silicane 10% with 900ml and carry out 20 minutes silanization.
To 4): similar embodiment 2.
Table 2
| Solvent | Topped degree r μ mol/m 2 | Conversion degree % |
| Normal heptane toluene carrene | 0.31 0.6 0.57 | 7.8 15.0 14.8 |
Table 3
| Solvation | Topped degree r μ mol/m 2 | Conversion degree % |
| 0.04%HCl in methyl alcohol 10% chloroacetic chloride in toluene 10% glacial acetic acid in toluene 10% propionic acid in toluene 10% trifluoracetic acid in toluene 10% trichloroacetic acid in toluene 10% dichloroacetic acid in toluene the 100g chloroacetic acid in 1 liter of toluene | 0.36 0.18 0.25 0.18 1.05 1.01 0.76 0.52 | 9.0 4.5 6.2 4.5 26.2 25.2 19.0 13.0 |
Table 4
| Chloroacetic chloride/10% glacial acetic acid in toluene 1: 93: 75: 56: 48: 29: 1 |
| Carbon percentage 14.5 10.2 6.9 6.5 6.2 6.1 |
Claims (15)
1, based on the parting material of the book layer chromatography that on carrier material, is coated with one deck adsorbent, mainly by after coating by the silanizing agent surface modification layer of silica gel formed, it is characterized in that, there is a uniform overcoat on the wettable silica gel surface of water, is 0.15～0.8 μ mol/m to reverse (RP) material a)
2Or b) be 1.2～2.5 μ mol/m to water wetted material
2
2, according to the parting material of the book layer chromatography of claim 1, it is characterized in that to being the anti-phase material of base with C18-alkyl chain (RP18), the even overcoat of the layer of silica gel that water is wettable is 0.3～0.5 μ mol/m
2
3, according to the parting material of the book layer chromatography of claim 1, it is characterized in that to being the anti-phase material of base with C8-alkyl chain (RP8), the even overcoat of the layer of silica gel that water is wettable is 0.35～0.7 μ mol/m
2
4, according to the parting material of the book layer chromatography of claim 1, it is characterized in that to water wetted material, the even overcoat of the layer of silica gel that water is wettable is 1.5～2.3 μ mol/m
2
5, based on carrier material, be coated with one deck adsorbent and by carry out the production method of the parting material that is used for the book layer chromatography of layer of silica gel surface modification with silanizing agent, it is characterized in that, before usefulness silanization material processed, the catalyst solution of the Silanization reaction of the capable catalysis silica gel of usefulness soaks evenly to be coated with wants silica gel surface modification, that water is wettable.
6, according to the method for claim 5, it is characterized in that, when being coated with, do not get rid of moisture with modification.
7, according to the method for claim 5, it is characterized in that,, use certain catalyst solution in view of by the modification of hope control surface.
According to the method for claim 7, it is characterized in that 8, catalyst concn is 0.01～20 weight % in soaking solution.
According to the method for claim 5, it is characterized in that 9, cleaning step is to remove unnecessary catalyst solution in the middle of will inserting one at least between coating and the modification.
10, according to the method for claim 5, it is characterized in that having 0.15～0.80 μ mol/m in order to produce
2The parting material of topped degree, use R-Six
3The silane of type, R is unsubstituted and the alkyl of 1～20 carbon atom is arranged in alkyl chain herein, aryl or aralkyl, x are alkoxyl or the alkyl that 1～20 carbon atom is arranged in alkyl chain, and to have an x at least be alkoxyl or aralkoxy.
According to the method for claim 5, it is characterized in that 11, it is 1.2～2.5 μ mol/m that production has topped degree
2Parting material the time use R-SiX
3The silane of type, herein
R represents alkyl, aryl or aralkyl, and each contains an epoxy radicals or amino at least,
X is illustrated in the alkoxyl or the alkyl of 1～20 carbon atom in the alkyl chain, and at least one X is alkoxyl or aralkoxy.
According to the method for claim 11, it is characterized in that 12, additional epoxy radicals is being converted into the dihydroxylic alcohols group by handling after the surface modification in diluted acid.
According to the method for claim 10, it is characterized in that 13, the mixed liquor of chloroacetic chloride and glacial acetic acid is used as catalyst.
14, according to the method for claim 11, it is characterized in that, trichloroacetic acid, dichloroacetic acid, chloroacetic acid or trifluoracetic acid, difluoro acetic acid, fluorine acetic acid is used as catalyst.
15, the parting material of producing according to the arbitrary method among the claim 5-14.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85105260 CN85105260A (en) | 1985-07-09 | 1985-07-09 | The parting material of thin-layered chromatography |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85105260 CN85105260A (en) | 1985-07-09 | 1985-07-09 | The parting material of thin-layered chromatography |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN85105260A true CN85105260A (en) | 1987-01-07 |
Family
ID=4794364
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 85105260 Pending CN85105260A (en) | 1985-07-09 | 1985-07-09 | The parting material of thin-layered chromatography |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN85105260A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304397C (en) * | 2005-04-07 | 2007-03-14 | 南京南大表面和界面化学工程技术研究中心有限责任公司 | Active alkylated silica gel and preparation method |
| CN102205234A (en) * | 2011-01-14 | 2011-10-05 | 安徽良臣硅源材料有限公司 | Preparation method for preparative thin layer chromatography silica gel plate with a layer thickness of 0.5-2.0 mm |
| CN103263785A (en) * | 2013-05-03 | 2013-08-28 | 西安交通大学 | Method for separating and purifying acidulous components by modified silica gel |
-
1985
- 1985-07-09 CN CN 85105260 patent/CN85105260A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304397C (en) * | 2005-04-07 | 2007-03-14 | 南京南大表面和界面化学工程技术研究中心有限责任公司 | Active alkylated silica gel and preparation method |
| CN102205234A (en) * | 2011-01-14 | 2011-10-05 | 安徽良臣硅源材料有限公司 | Preparation method for preparative thin layer chromatography silica gel plate with a layer thickness of 0.5-2.0 mm |
| CN102205234B (en) * | 2011-01-14 | 2013-01-02 | 安徽良臣硅源材料有限公司 | Preparation method for preparative thin layer chromatography silica gel plate with a layer thickness of 0.5-2.0 mm |
| CN103263785A (en) * | 2013-05-03 | 2013-08-28 | 西安交通大学 | Method for separating and purifying acidulous components by modified silica gel |
| CN103263785B (en) * | 2013-05-03 | 2015-04-29 | 西安交通大学 | Method for separating and purifying acidulous components by modified silica gel |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US5326738A (en) | Stable, covalently-bonded supports for chemical separation apparatus made through a hydride intermediate | |
| AU2005291937A1 (en) | pH stable chromatographic media using templated multilayer organic/inorganic grafting | |
| JPH0623266A (en) | Complex polytetrafluoroethylene article having controlled cavity and its control method | |
| IL44300A (en) | Process for the chemical modification of surfaces of inorganic solids | |
| JP2001506364A (en) | Preformed polymer coating method and product | |
| CN1901990A (en) | Polar silanes for binding to substrates and use of the bound substrates in chromatography | |
| CN1213799C (en) | Sequential porous silica gel whole column and its preparation and use | |
| CN85105260A (en) | The parting material of thin-layered chromatography | |
| EP0572907A2 (en) | Chemically synthesized silanes that bind nucleic acids | |
| EP0170143A2 (en) | Separation materials for thin-layer chromatography | |
| CN1204401A (en) | Packing material for high-speed liquid chromatography | |
| GB2190369A (en) | Reversed-phase packing material and method | |
| WO2004046714A1 (en) | Separating agent for optical isomer | |
| US5869724A (en) | Asymmetric bidentate silanes | |
| CN1758959A (en) | Separating agent for optical isomer | |
| CN1130375A (en) | Separating agent for optical isomers | |
| CN1712967A (en) | Silicon rubber micro-fluid control chip with polyvinyl alcohol surface coating and surface modification thereof | |
| CN1281750A (en) | Shape selective modification method of zeolite catalyst | |
| WO1984004913A1 (en) | Method for reducing the hydrocarbon content in air or water | |
| EP1559684A1 (en) | Method of separating a substance from a liquid | |
| JPS6310785B2 (en) | ||
| CN1099034C (en) | Filler for high-performance liquid chromatography and method of manufacturing the same | |
| US20160077068A1 (en) | Thin-layer chromatography plate, method for producing such a plate, and method for performing a thin-layer chromatography separation | |
| CA2360322C (en) | New hydrophobic polymer comprising fluorine moieties | |
| GB1580675A (en) | Separation material for thin layer chromatography |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |