CN102205234B - Preparation method for preparative thin layer chromatography silica gel plate with a layer thickness of 0.5-2.0 mm - Google Patents
Preparation method for preparative thin layer chromatography silica gel plate with a layer thickness of 0.5-2.0 mm Download PDFInfo
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- CN102205234B CN102205234B CN 201110008709 CN201110008709A CN102205234B CN 102205234 B CN102205234 B CN 102205234B CN 201110008709 CN201110008709 CN 201110008709 CN 201110008709 A CN201110008709 A CN 201110008709A CN 102205234 B CN102205234 B CN 102205234B
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- silica gel
- gel plate
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- mix monomer
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- 239000000203 mixture Substances 0.000 claims 7
- 239000000178 monomer Substances 0.000 claims 6
- 238000006243 chemical reaction Methods 0.000 claims 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 4
- 239000011230 binding agent Substances 0.000 claims 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims 2
- 238000001035 drying Methods 0.000 claims 2
- 239000008240 homogeneous mixture Substances 0.000 claims 2
- 229910052757 nitrogen Inorganic materials 0.000 claims 2
- 239000000047 product Substances 0.000 claims 2
- 239000000741 silica gel Substances 0.000 claims 2
- 229910002027 silica gel Inorganic materials 0.000 claims 2
- 239000007787 solid Substances 0.000 claims 2
- 239000000758 substrate Substances 0.000 claims 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims 1
- OELQSSWXRGADDE-UHFFFAOYSA-N 2-methylprop-2-eneperoxoic acid Chemical compound CC(=C)C(=O)OO OELQSSWXRGADDE-UHFFFAOYSA-N 0.000 claims 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims 1
- 229920004933 Terylene® Polymers 0.000 claims 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims 1
- 239000000853 adhesive Substances 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 claims 1
- 239000005030 aluminium foil Substances 0.000 claims 1
- 238000003556 assay Methods 0.000 claims 1
- 238000001816 cooling Methods 0.000 claims 1
- 238000004090 dissolution Methods 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 239000011521 glass Substances 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000000034 method Methods 0.000 claims 1
- 239000003960 organic solvent Substances 0.000 claims 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims 1
- 239000005020 polyethylene terephthalate Substances 0.000 claims 1
- 238000006116 polymerization reaction Methods 0.000 claims 1
- 239000002244 precipitate Substances 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- 238000012746 preparative thin layer chromatography Methods 0.000 claims 1
- 125000004368 propenyl group Chemical group C(=CC)* 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- 238000010792 warming Methods 0.000 claims 1
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- Cosmetics (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a preparation method for a preparative thin layer chromatography (TLC) silica gel plate with a layer thickness of 0.5-2.0 mm, and belongs to chromatographic separation technology. The preparation method comprises steps of uniformly mixing a TLC silica gel and a novel adhesive; coating the resulting mixture on a glass substrate, an aluminium foil substrate or a terylene substrate through a coater; putting the coated substrate into a drying oven and carrying out a drying process to prepare the TLC silica gel plate. The TLC silica gel plate has advantages of a layer thickness of 0.5-2.0 mm, a flat and smooth substrate surface, strong green light, a uniform and firm thin layer, no crack, no shallow crackle, no falling off, autonomic regulation of the layer thickness between 0.5-2.0 mm, a nonparallelism less than or equal to 0.02 mm, a qualified rate higher than or equal to 99.5%. The silica gel plate is used under normal temperature and pressure, and has advantages of simplicity, fastness and high efficiency. The silica gel plate is widely applicable for a plurality of fields such as drug industry, biotechnology, biomedicine and biochemistry, energy, food, cosmetics, environmental science, natural product chemistry.
Description
Technical field
The present invention relates to a kind of preparation method of 0.5-2.0mm preparative thin-layer chromatography silica gel plate, belong to chemical field.
Background technology
Chromatogram be so far human grasp to the complex mixture analysis, separate effective method, the thin-layer chromatography silica gel plate (or claims the tlc silica gel plate, thickness of thin layer 0.2-0.25mm, TLC) be widely used in that organic synthesis, medicine are synthetic, the analysis of the active ingredient in the natural product chemistry, has simple, fast and efficient analysis characteristic, certainly, this thin-layer chromatography silica gel plate also is applicable to the separation of micro-example, if increase the thickness of thin layer, its volume containing the sample and separated object will increase greatly.Usually, people are with thickness of thin layer 0.2-0.25mm thin-layer chromatography silica gel plate, be called analysis plates, thickness of thin layer 0.3-0.4mm is called accurate preparation plate, and thickness of thin layer 0.5-2.0mm is called the preparation plate, therefore, the Merck KGaA company nineties in last century (MERCK) develop goes out thickness of thin layer 0.5-2.0mm preparative scale chromatography silica gel plate (PTLC).
The preparative scale chromatography silica gel plate has precision height, fireballing separation characteristic, in organic synthesis, medication chemistry, biochemical technology separate with bioengineering, biologically active and the aspect such as natural products effective ingredient separation and purification has become the means that more and more important preparation separates, in many situations, required high-purity standard sample can only obtain with the preparative chromatography technology, such as the separation of racemic modification.Along with bioengineering and the modern active demand of traditional Chinese medicine, and in relevant field separation and purification tasks of the amount of facing all, the preparative scale chromatography silica gel plate has caused the great attention of countries in the world as a kind of isolation technics rapidly and efficiently.Along with the mankind to improving constantly that pharmaceutical purity requires, the preparative chromatography technology will become one of topmost method in the medicine purification and separation field owing to have the unrivaled characteristics of other isolation technics and powerful separating power.This technology is put in the brainstorm project of " 863 " engineering biological technical field in China.Wherein the preparative thin-layer chromatography silica gel plate is current people's most study, most widely used preparative thin-layer chromatography product, the preparative thin-layer chromatography silica gel plate (PTLC) of the 0.50-2.0mm that Merck KGaA company (MERCK) produces, because expensive, domestic common laboratory is seldom bought use, this limits domestic organic synthesis undoubtedly, medication chemistry, research and production means in biochemical technology and the molecular bioengineering, reduce research and production efficient, thereby, the preparative thin-layer chromatography silica gel plate (PTLC) of development 0.50-2.0mm has urgency and urgency, it can fill the domestic gaps, also can export goods and earn foreign currency, will have far reaching significance.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of 0.5-2.0mm preparative thin-layer chromatography silica gel plate, to solve the deficiencies in the prior art, make things convenient for the better separation and Extraction of chemical constituent.
The present invention adopts following technical scheme to achieve these goals:
0.5-2.0mm the preparation method of preparative thin-layer chromatography silica gel plate is characterized in that may further comprise the steps:
(1) tlc silica gel and 0.5-1.0% binder solution are evenly mixed, form preferably homogeneous mixture of levelability; The ratio of general tlc silica gel and 0.5-1.0% binder solution weight is 100: 20.
(2) homogeneous mixture is coated on the bright and clean base plate, comprises the substrate of glass, aluminium foil, terylene, thickness of thin layer is controlled at 0.5-2.0mm;
(3) substrate is put into thermostatic drying chamber, and baking temperature is controlled at 105-110 ℃, 2-3 hour drying time;
(4) after the product oven dry, be cooled to room temperature;
(5) product is packed warehouse-in through after the assay was approved.
Described preparation method is characterized in that described adhesive is that acrylic acid and derivative copolymerization thereof form.
Described preparation method is characterized in that described adhesive prepares by the following method:
(1) in reactor, adds reaction dissolvent, with air in the nitrogen replacement reactor, under nitrogen protection, open and stir;
(2) add the mixture of small part (1/3) mix monomer and initator in the reactor, be warming up to 90 ℃, initiated polymerization;
(3) drip remaining major part (2/3) mix monomer, reaction temperature is controlled in 97 ℃, continues reaction, and residual monomer is reacted completely;
(4) with mixture cooling after step (3) reaction, in the impouring ethanolic solution, get the graininess precipitation;
(5) filtering precipitate is placed in the baking oven and dries, and namely gets solid binder;
(6) with the solid binder organic solvent dissolution that makes, obtain the 0.5-1.0% binder solution;
Each components by weight of described mix monomer: methacrylic acid hydroxyl ester: propenyl: acrylamide=10: 60: 30;
Described initator is selected persulfate, azodiisobutyronitrile, in hydrogen peroxide-ferrous salt one or more, consumption is the 0.2-0.3% of mix monomer weight;
Described reaction dissolvent is one or more in dimethyl formamide, oxolane, the ethanol, and consumption is 4-5 times of mix monomer weight.
Beneficial effect of the present invention:
The thin-layer chromatography silica gel plate that the present invention makes, thickness of thin layer 0.5-2.0mm, the plate face smooth smooth, fluorescence is emerald green bright, thin layer is even firmly, nothing chaps, shallow splitting and obscission, 0.5-2.0mm from main regulation, nonparallelism≤0.02mm, qualification rate is not less than 99.5%.Use under the normal temperature and pressure, have the advantages such as simple, quick, efficient, be widely used in the numerous areas such as pharmaceuticals industry, biotechnology, biomedicine and biochemistry, the energy, food, cosmetics, environmental science, natural product chemistry.
Description of drawings
Fig. 1 is the preparation flow figure of 0.5-2.0mm preparative thin-layer chromatography silica gel plate.
The specific embodiment
1, adhesive:
Adhesive is that acrylic acid and derivative copolymerization thereof form, and polymerization single polymerization monomer is multipolymer.This adhesive contains functional group such as carboxyl, hydroxyl, and cyano group, ehter bond, the vinylation polymerisation of the vinylation unsaturated monomer of glycidyl prepares.Functional monomer commonly used has acrylamide, propenyl, acrylonitrile, acrylic acid, methacrylic acid, acrylate, crylic acid hydroxy ester, methacrylic acid hydroxyl ester, vinyl acetate, styrene etc.
Initator: persulfate, azodiisobutyronitrile, hydrogen peroxide-ferrous salt etc.
Reaction dissolvent: dimethyl formamide (DMF), oxolane (THF), ethanol etc.
2, a kind of preparation of adhesive:
Thin-layer chromatography silica gel (or tlc silica gel) can be bought from market, meet HG/T 2354-1992 index, adhesive acrylic acid derivative type (self-control), substrate is 1.5-2.0mm glass plate, aluminium foil, terylene plate etc., the bed board device is Switzerland CAMAG automatic coating plate paver, baking oven is constant temperature numerical control baking oven (25-300 ℃), and thickness is counted the ZBH-4 thickness gauge.
In the reactor that heating jacket, electric mixer, thermometer, reflux condenser are housed, add a certain amount of solvent dimethylformamide; under nitrogen protection, open and stir; with air displacement in the reactor three times, add the mixture of 1/3 mix monomer and initator, be warming up to 90 ℃; initiated polymerization 0.5 hour; then, drip remaining mix monomer, reaction temperature is controlled in 97 ℃; continue reaction 3 hours, residual monomer is reacted completely.When then being cooled to 40 ℃, in reactant mixture impouring 70% ethanolic solution, get the graininess precipitation.Leach sediment, be placed in the baking oven and dry, namely get solid binder.With the solid binder acetone solution that makes, obtain about 0.5-1.0% binder solution.
Each components by weight in the mix monomer: methylacrylic acid hydroxy ester: propenyl: acrylamide=10: 60: 30.
Initator: azodiisobutyronitrile is 0.3% of mix monomer weight.
Dimethyl formyl solvent: for the 4-5 of mix monomer weight doubly.
3, preparative thin-layer chromatography silica gel plate:
The 0.5-1.0% binder solution of thin-layer chromatography silica gel (or tlc silica gel) and (1) or (2) evenly mixes, obtain preferably mixture of levelability, adopt coating machine that homogeneous mixture is coated with and be layered on glass, on the substrate such as aluminium foil or terylene, it is dry to put into baking oven, make thin-layer chromatography silica gel plate (or tlc silica gel plate), thickness of thin layer scope 0.5-2.0mm, it is dry that wet plate is put into constant temperature oven, baking temperature is controlled at 105-110 ℃, about 2-3 hour drying time, after the product oven dry, be cooled to room temperature, in baking oven, take out product.The plate face smooth smooth, thickness of thin layer is even, thin layer is firm, without be full of cracks, shallow splitting and obscission, and the fluorescence kingfisher is bright, 0.5-2.0mm is from main regulation, nonparallelism≤0.02mm, qualification rate is not less than 99.5%.
Technical indicator:
Thickness of thin layer: 0.5-2.0mm.
Activity: (to the separation of indigo, tonyred, dimethyl yellow) three looks obviously separate.
Thin layer adhesive fastness: the cutting of useable glass cutter and pencil writing mark.
Tlc silica gel: meet HG/T 2354-1992 index.
Anti-detect interference: on sulfuric acid and potassium permanganate without impact.
PH value: 6.2-6.8.
Main Types: G type, GF254 type, GF365 type, H type, HF254 type, HF365 type.
Main specifications: 200x200mm, 100x200mm.
Claims (1)
1. the preparation method of a 0.5-2.0mm preparative thin-layer chromatography silica gel plate is characterized in that may further comprise the steps:
(1) tlc silica gel and 0.5-1.0% binder solution are evenly mixed, form preferably homogeneous mixture of levelability;
(2) homogeneous mixture is coated on the bright and clean base plate, described base plate is the substrate of glass, aluminium foil, terylene, and thickness of thin layer is controlled at 0.5-2.0mm;
(3) substrate is put into thermostatic drying chamber, and baking temperature is controlled at 105-110 ℃, 2-3 hour drying time;
(4) after the product oven dry, be cooled to room temperature;
(5) product is packed warehouse-in through after the assay was approved; Described adhesive prepares by the following method:
(1) in reactor, adds reaction dissolvent, with air in the nitrogen replacement reactor, under nitrogen protection, open and stir;
(2) add the mixture of small part mix monomer and initator in the reactor, be warming up to 90 ℃, initiated polymerization;
(3) drip remaining most of mix monomer, reaction temperature is controlled in 97 ℃, continues reaction, and residual monomer is reacted completely;
(4) with mixture cooling after step (3) reaction, in the impouring ethanolic solution, get the graininess precipitation;
(5) filtering precipitate is placed in the baking oven and dries, and namely gets solid binder;
(6) with the solid binder organic solvent dissolution that makes, obtain the 0.5-1.0% binder solution;
Each components by weight of described mix monomer: methacrylic acid hydroxyl ester: propenyl: acrylamide=10: 60: 30;
Described initator is selected persulfate, azodiisobutyronitrile, in hydrogen peroxide-ferrous salt one or more, consumption is the 0.2-0.3% of mix monomer weight;
Described reaction dissolvent is one or more in dimethyl formamide, oxolane, the ethanol, and consumption is 4-5 times of mix monomer weight.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110008709 CN102205234B (en) | 2011-01-14 | 2011-01-14 | Preparation method for preparative thin layer chromatography silica gel plate with a layer thickness of 0.5-2.0 mm |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110008709 CN102205234B (en) | 2011-01-14 | 2011-01-14 | Preparation method for preparative thin layer chromatography silica gel plate with a layer thickness of 0.5-2.0 mm |
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| CN102205234A CN102205234A (en) | 2011-10-05 |
| CN102205234B true CN102205234B (en) | 2013-01-02 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106053705B (en) * | 2016-07-22 | 2018-01-16 | 黄石科森色谱科技有限公司 | A kind of preparation method of reverse-phase chromatography plate |
| CN109932471A (en) * | 2019-03-12 | 2019-06-25 | 南开大学 | A kind of method of fast laying thin layer chromatography plate |
| 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 |
| CN113462326A (en) * | 2021-07-01 | 2021-10-01 | 烟台工程职业技术学院(烟台市技师学院) | Preparation and application method of reverse-phase thin-layer chromatography silica gel plate adhesive |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85105260A (en) * | 1985-07-09 | 1987-01-07 | 默克专利股份有限公司 | The parting material of thin-layered chromatography |
| US5670631A (en) * | 1992-05-26 | 1997-09-23 | Thomas Bayerl | Procedure of separation of proteins by column chromatography using silica gels coated by a lipid bilayer |
| CN101161679A (en) * | 2007-11-01 | 2008-04-16 | 江南大学 | Method for preparing dexamethasone artificial antigen |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002320834A (en) * | 2001-04-26 | 2002-11-05 | Tdk Corp | Silica gel membrane and method for producing the same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85105260A (en) * | 1985-07-09 | 1987-01-07 | 默克专利股份有限公司 | The parting material of thin-layered chromatography |
| US5670631A (en) * | 1992-05-26 | 1997-09-23 | Thomas Bayerl | Procedure of separation of proteins by column chromatography using silica gels coated by a lipid bilayer |
| CN101161679A (en) * | 2007-11-01 | 2008-04-16 | 江南大学 | Method for preparing dexamethasone artificial antigen |
Non-Patent Citations (1)
| Title |
|---|
| JP特开2002-320834A 2002.11.05 |
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