CN102336869A - Preparation method of methimazole molecularly imprinted polymer - Google Patents
Preparation method of methimazole molecularly imprinted polymer Download PDFInfo
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- CN102336869A CN102336869A CN2010102324948A CN201010232494A CN102336869A CN 102336869 A CN102336869 A CN 102336869A CN 2010102324948 A CN2010102324948 A CN 2010102324948A CN 201010232494 A CN201010232494 A CN 201010232494A CN 102336869 A CN102336869 A CN 102336869A
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- molecularly imprinted
- thiamazole
- imprinted polymer
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Abstract
The invention relates to a preparation method of a methimazole molecularly imprinted polymer. The method comprises the technical key points of: dissolving the template molecule methimazole, the functional monomer methacrylic acid and the cross-linking agent ethylene glycol dimethacrylate in a mole ratio of 1:4:5.81 into the pore forming agent absolute ethanol; adding the initiator azodiisobutyronitrile, conducting ultrasonic processing for 20min, introducing nitrogen for 15min, initiating polymerization under ultraviolet irradiation (lambda=365nm) for 12h; after the reaction, crushing and sieving the product, and taking polymer particles with a particle size of 80-125 micrometers, and washing the particles with a mixed solution of 50mL of methanol and 50mL 1.0mol L<-1> of hydrochloric acid under stirring, carrying out soxhlet extraction with a mixed solution of methanol and glacial acetic acid that are in a volume ratio of 9:1 to remove the template molecule, implementing vacuum drying at a temperature of 70DEG C for 10h, thus obtaining the methimazole molecularly imprinted polymer. The preparation method of the invention has low cost, simple synthesis process and easily controllable reaction conditions, and the obtained molecularly imprinted polymer can be used for concentration of the trace amount of methimazole existing in a sample and substrate purification, so that the method provided in the invention boasts great application value and market prospects.
Description
Technical field
The present invention relates to technical field of polymer materials, relate in particular to a kind of preparation method of Thiamazole molecularly imprinted polymer.
Background technology
Thiamazole (Methimazole) belongs to ATD, is mainly used in treatment hyperthyroidism clinically.Its mechanism of action is to hinder the oxidation of iodide in the Tiroidina and the coupling of tyrosine through suppressing the activity of Tiroidina endoperoxide enzyme, hinders the synthetic of thyroxine (T4) and trilute (T3).It is reported, take in biological intravital Thiamazole 79.2% and excrete with the form of former medicine, but remainder branch remains in the tissue, the metabolism of life entity is had side effects, like dermatitis, sense of taste sense of smell is become deaf, pharyngitis, high fever or the like.Ephritis can appear in the minority case, the illness that hepatitis etc. are comparatively serious.The method that the domestic and international at present method at the detection Thiamazole mainly concentrates on chromatography or chromatogram and mass spectrometry is carried out qualitative, quantitative detection, and test sample is generally urine sample, serum, muscle tissue etc.But because the complicacy of sample substrate, aforesaid method needs comparatively loaded down with trivial details sample pretreatment process in testing process, adopts usually fast, simple solid phase extraction techniques.And the filler of traditional SPE is normally nonspecific to the absorption of analyte, is unfavorable for the purification of sample.Molecular imprinting is a kind of based on the chemical polymerization thing technology of preparing on the molecular recognition basis, is one of main method of current preparation high selectivity material.Because prepared polymkeric substance has " memory " function, can have an effect with template molecule specifically, and can elute through certain mode, thereby reach the effect of purifying and enrichment target molecule.And because its environment is practical, repeatable high characteristics have shown application promise in clinical practice at the surface side filler of SPE.
Summary of the invention
The objective of the invention is to overcome prior art deficiency, a kind of preparation method of the molecular engram material to Thiamazole highly selective absorption is provided; This molecularly imprinted polymer can be used for the stationary phase of SPE, directly is used for the separation and the detection of Thiamazole.Technical scheme of the present invention is:
(1) be Thiamazole, function monomer methylacrylic acid and linking agent ethylene glycol dimethacrylate according to molar ratio with template molecule be to be dissolved into the pore-creating agent absolute ethyl alcohol at 1: 4: 5.81.When the amount of substance of template molecule was 2.19mmol, the volume of described pore-creating agent was 10mL.Add Diisopropyl azodicarboxylate;
(2) ultrasonic 20min slowly feeds nitrogen 15min, UV-irradiation (the initiated polymerization 12h of λ=365nm).After reaction finished, product was got the polymer beads that size is 80-125 μ m through pulverizing, sieving;
(3) with the polymkeric substance that makes with 50mL methyl alcohol and 50mL 1.0mol L
-1The mixing solutions agitator treating 6h of hydrochloric acid, the use volume ratio is that methyl alcohol-glacial acetic acid mixing solutions Suo Shi of 9: 1 extracts 24h, further removes template molecule, then at 70 ℃ of vacuum-drying 10h, promptly obtains Thiamazole is had the sorbing material of highly selective.
Advantage of the present invention and positively effect are:
(1) Thiamazole molecular engram material provided by the invention is that template molecule is synthetic with the Thiamazole, and single-minded identification Thiamazole has very high selectivity; This material prepares with chemical synthesis process, and advantages of higher stability, the work-ing life of growing and stronger anti-adverse environment ability are arranged.
(2) the present invention is with low cost; Experimental implementation is simple, easy control of reaction conditions, and imprinted sites is stable in the Thiamazole molecularly imprinted polymer that makes; Can be used as sorbent material and be used for SPE and liquid chromatography coupling, be applicable to enrichment of trace Thiamazole and sample purification in the various samples.
Embodiment
Below in conjunction with embodiment, the present invention is further specified; Following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
The present invention utilizes the synthetic adsorption functional material that Thiamazole is had highly selective of molecular imprinting, and its specific embodiment is:
(1) accurately measures absolute ethyl alcohol 10.0mL and place round-bottomed flask; Get Thiamazole 2.19mmol, methylacrylic acid 8.78mmol, ethylene glycol dimethacrylate 12.68mmol, stirring reaction 2h; Add Diisopropyl azodicarboxylate 130mg; Ultrasonic 20min slowly feeds nitrogen 15min, UV-irradiation (the initiated polymerization 12h of λ=365nm);
(2) above-mentioned polymerisate process is pulverized, sieved, get the polymer beads that size is 80-125 μ m;
(3) with the polymkeric substance that makes with 50mL methyl alcohol and 50mL 1.0mol L
-1The mixing solutions agitator treating 6h of hydrochloric acid, the use volume ratio is that methyl alcohol-glacial acetic acid mixing solutions Suo Shi of 9: 1 extracts 24h, further removes template molecule;
(4) polymkeric substance that will remove template molecule obtains the Thiamazole molecularly imprinted polymer at 70 ℃ of vacuum-drying 10h.
Claims (7)
1. the preparation method of a Thiamazole molecularly imprinted polymer is characterized in that, comprises the steps:
1) be Thiamazole, function monomer methylacrylic acid and linking agent ethylene glycol dimethacrylate according to molar ratio with template molecule is to be dissolved in pore-creating agent absolute ethyl alcohol at 1: 4: 5.81, adds the initiator Diisopropyl azodicarboxylate;
2) ultrasonic 20min slowly feeds nitrogen 15min, UV-irradiation (the initiated polymerization 12h of λ=365nm).After reaction finished, product was got the polymer beads that size is 80-125 μ m through pulverizing, sieving;
3) with 50mL methyl alcohol and 50mL 1.0mol L
-1The mixing solutions agitator treating 6h of hydrochloric acid, the use volume ratio is that methyl alcohol-glacial acetic acid mixing solutions Suo Shi of 9: 1 extracts 24h, further removes template molecule;
4) polymkeric substance that will remove template molecule obtains the Thiamazole molecularly imprinted polymer at 70 ℃ of vacuum-drying 10h;
2. the preparation method of a kind of Thiamazole molecularly imprinted polymer according to claim 1 is characterized in that: when the amount of substance of template molecule was 2.19mmol, the volume of described pore-creating agent was 10mL;
3. the preparation method of a kind of Thiamazole molecularly imprinted polymer according to claim 1 is characterized in that: described pore-creating agent composition is an absolute ethyl alcohol;
4. the preparation method of a kind of Thiamazole molecularly imprinted polymer according to claim 1 is characterized in that: the molar ratio of described template molecule, function monomer and linking agent is 1: 4: 5.81;
5. the preparation method of a kind of Thiamazole molecularly imprinted polymer according to claim 1 is characterized in that: the ratio of described linking agent and Diisopropyl azodicarboxylate is 16: 1;
6. the preparation method of a kind of Thiamazole molecularly imprinted polymer according to claim 1 is characterized in that: described washing copolymer particulate mixing solutions is methyl alcohol and 1.0mol L
-1The mixed solution of hydrochloric acid, volume ratio are 1: 1, and washing time is 6h;
7. the preparation method of a kind of Thiamazole molecularly imprinted polymer according to claim 1 is characterized in that: described soxhlet extraction solvent is the mixed solution of methyl alcohol and glacial acetic acid, and volume ratio is 9: 1, and the soxhlet extraction time is 24h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102324948A CN102336869A (en) | 2010-07-21 | 2010-07-21 | Preparation method of methimazole molecularly imprinted polymer |
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| CN2010102324948A CN102336869A (en) | 2010-07-21 | 2010-07-21 | Preparation method of methimazole molecularly imprinted polymer |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103396512A (en) * | 2013-07-24 | 2013-11-20 | 河北科技大学 | Hybrid template molecularly imprinted polymer as well as preparation method and application of hybrid template molecularly imprinted solid-phase extraction column |
| CN105486869A (en) * | 2014-10-08 | 2016-04-13 | 江苏维赛科技生物发展有限公司 | Enzyme linked immunosorbent assay kit for detecting methimazole residues in animal-derived food and application thereof |
| CN106674425A (en) * | 2016-11-29 | 2017-05-17 | 湖北大学 | Preparation method for nanoparticle capable of releasing vancomycin by responding to pH |
-
2010
- 2010-07-21 CN CN2010102324948A patent/CN102336869A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103396512A (en) * | 2013-07-24 | 2013-11-20 | 河北科技大学 | Hybrid template molecularly imprinted polymer as well as preparation method and application of hybrid template molecularly imprinted solid-phase extraction column |
| CN103396512B (en) * | 2013-07-24 | 2016-02-03 | 河北科技大学 | The preparation method and application of hybrid template molecularly imprinted polymer and solid-phase extraction column thereof |
| CN105486869A (en) * | 2014-10-08 | 2016-04-13 | 江苏维赛科技生物发展有限公司 | Enzyme linked immunosorbent assay kit for detecting methimazole residues in animal-derived food and application thereof |
| CN106674425A (en) * | 2016-11-29 | 2017-05-17 | 湖北大学 | Preparation method for nanoparticle capable of releasing vancomycin by responding to pH |
| CN106674425B (en) * | 2016-11-29 | 2019-04-30 | 湖北大学 | A kind of preparation method of the nanosphere of pH response Vancomycin |
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