CN102382248A - Preparation method of chlorsulfuron molecular imprinting polymer - Google Patents
Preparation method of chlorsulfuron molecular imprinting polymer Download PDFInfo
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- CN102382248A CN102382248A CN2010102727224A CN201010272722A CN102382248A CN 102382248 A CN102382248 A CN 102382248A CN 2010102727224 A CN2010102727224 A CN 2010102727224A CN 201010272722 A CN201010272722 A CN 201010272722A CN 102382248 A CN102382248 A CN 102382248A
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- chlorine sulphur
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Abstract
The invention relates to a preparation method of chlorsulfuron molecular imprinting polymer which purely adopts ionic liquid as a single function body. The preparation method is mainly technically characterized in that chlorsulfuron is used as a template molecule, ionic liquid chlorination 1- vinyl-3-butyl imidazole is used as the single function body, glycol dimethyl acrylic ester is used as cross linking agent, N and N- dymethyl formamide is used as porogenic agent, toluene is used as liquor, and the high-selectivity chlorsulfuron molecular imprinting polymer is synthesized by the aid of the polymer preparation method. The preparation method is low in cost, a synthesis process is simple, reaction conditions are easy to control, the prepared chlorsulfuron molecular imprinting polymer is fine in adsorption effect, and the preparation method is suitable for adsorption detection of chlorsulfuron in food and has wide application prospect.
Description
Technical field
The present invention relates to technical field of polymer materials, relate in particular to the preparation method of the grand molecularly imprinted polymer of a kind of chlorine sulphur.
Background technology
Chlorine sulphur grand (chlorsulforon is called for short CS) is a kind of sulfonylurea herbicide of du pont company exploitation, and this compound activity is high; Consumption is extremely low; Broad weed-killing spectrum can be invaded body through respiratory tract, digestive tube, also can be through mucocutaneous slow absorption; Mainly be distributed in liver, kidney, fat and the muscle tissue, drain slowly in vivo.Result of study shows, chlorine sulphur swells rat oral LD
505545mg/kg, rabbit is acute through skin LD
503400mg/kg belongs to the lower toxicity agricultural chemicals.Cumulative toxicity test is the result show, this medicine has tangible cumulative effect in animal body, and 90 days subchronic tests think that tentatively its maximum no-effect dose is 100mg/kg.Adopt 3H mark tracer method to the grand pharmacokinetic that carried out of chlorine sulphur, the result shows after 3H chlorine sulphur swells in digestive tube gets into animal body and can absorb rapidly, is distributed to whole body, and can sees through hemato encephalic barrier.This medicine is drained slowly in vivo, and no mutagenesis does not find to have tangible teratogenic effect.The animal cell immunity function is had restraining effect, but the influence of pair cell immune organ is not obvious.Toxic action mechanism is inquired into the result and is shown that chlorine sulphur swells in the liver metabolism process, and the biological oxidation of pair cell has certain influence.
At present, the foreign study person is more to the residual research of sulfonylurea herbicide in soil and tap water, and domestic present residual limit the quantity of and corresponding standard detection method of such weedicide in surrounding medium of not formulating as yet.According to European Union's tap water criterion, (to single agricultural chemicals, the detectable level that requires analytical procedure is less than 0.1 μ g/L; Require detectable level less than 0.5 μ g/L to the agricultural chemicals total amount), stipulated that the LOQ value of the residual measuring method of sulfonylurea herbicide is 0.05 μ g/L in the tap water.Proposed many sulfonylurea herbicide residue analysis methods at present, summed up and to get up to be divided into three major types: be i.e. enzymoimmunoassay, bioassay method and instrumental method.Wherein, instrument analytical method can be proved conclusively detected result, but need with the coupling of some separation and concentrations technology, to reach detection requirement to the different sources analytic target.Molecular imprinting is one of main method of current preparation high selectivity material; Prepared polymkeric substance has shown application promise in clinical practice at aspects such as SPE, clinical medicine analysis, mimetic enzyme catalysis, Biomimic electrodes; Institute's synthetic polymer stabilizing; Selectivity is higher, can be widely used in the grand on-line selection absorption of trace amounts of chlorine sulphur and detect.
Summary of the invention
The object of the present invention is to provide the preparation method of the grand molecularly imprinted polymer of a kind of chlorine sulphur, the molecularly imprinted polymer that makes with this method has highly selective to chlorine sulphur is swelled, and technical scheme of the present invention is:
(1) at N, add the grand and ionic liquid chlorination 1-vinyl-3-NSC 158165 of chlorine sulphur in dinethylformamide and the toluene solvant, add methyl alcohol then, ultrasonic promotion dissolving.The dark place is left standstill and is added the linking agent ethylene glycol dimethacrylate after 4 hours; Add the initiator Diisopropyl azodicarboxylate, 60 ℃ of water-bath thermopolymerization 24h behind the ultrasonic and logical nitrogen;
(2) bulk polymer that makes being used the volume ratio of methyl alcohol and glacial acetic acid is extract extracting 24h in apparatus,Soxhlet's of 9: 1, and vacuum-drying 10～12h under 60 ℃ of temperature condition promptly obtains the grand high selection adsorption functional material of chlorine sulphur then.
Advantage of the present invention and positively effect are:
(1) the grand molecular engram material of chlorine sulphur provided by the invention is grand with chlorine sulphur is that template molecule is synthetic, and single-minded identification chlorine sulphur is grand, 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, and experimental implementation is simple, easy control of reaction conditions, and the grand molecularly imprinted polymer of the chlorine sulphur that makes is used for SPE and liquid chromatography coupling as sorbent material, is applicable to grand online detection and the sample purification of trace amounts of chlorine sulphur in the food.
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 is to be independent function monomer with ionic liquid, and synthetic have the highly selective adsorption functional material to chlorine sulphur is grand, and its specific embodiment is:
(1) the 7.4g 1-chlorobutane is dropwise added 4g 1-vinyl imidazole, under 70 ℃ condition, magnetic agitation reaction 50h.Be separated after reacting completely, product is a viscous liquid, with the ETHYLE ACETATE repetitive scrubbing repeatedly.The product that obtains at room temperature carries out vacuum-drying to constant weight, promptly obtains product ion liquid chlorination 1-vinyl-3-NSC 158165 (ViBuIm
+Cl
-);
(2) at 2.5mL N, in dinethylformamide and the 4mL toluene, the grand template of adding 537mg chlorine sulphur fully stirs it is dissolved fully, adds the above-mentioned ionic liquid of 0.6795g then, adds 1mL methyl alcohol, and ultrasonic 5min promotes fully to dissolve; The dark place is left standstill and is added 1509 μ L linking agent ethylene glycol dimethacrylates after 4 hours; Add the 20mg Diisopropyl azodicarboxylate, ultrasonic 2min, logical nitrogen 10min seals rapidly, then 60 ℃ of water-bath thermopolymerization 24h;
(3) bulk polymer that makes being used the volume ratio of methyl alcohol and glacial acetic acid is extract extracting 24h in apparatus,Soxhlet's of 9: 1, and vacuum-drying 10～12h under 60 ℃ of temperature condition promptly obtains the grand high selection adsorption functional material of chlorine sulphur then.
Claims (3)
1. the preparation method of the grand molecularly imprinted polymer of a chlorine sulphur is characterized in that:
1) the 7.4g 1-chlorobutane is dropwise added 4g 1-vinyl imidazole, under 70 ℃ condition, magnetic agitation reaction 50h.Be separated after reacting completely, product is a viscous liquid, with the ETHYLE ACETATE repetitive scrubbing repeatedly.The product that obtains at room temperature carries out vacuum-drying to constant weight, promptly obtains product ion liquid chlorination 1-vinyl-3-NSC 158165 (ViBuIm+Cl-);
2) with the grand N that adds of chlorine sulphur, in dinethylformamide and the toluene, fully stirring is dissolved it fully, adds above-mentioned ionic liquid then, adds methyl alcohol, and ultrasonic promotion is fully dissolved; The dark place is left standstill and is added the linking agent ethylene glycol dimethacrylate after 4 hours; Add the initiator Diisopropyl azodicarboxylate, 60 ℃ of water-bath thermopolymerization 24h behind the ultrasonic and logical nitrogen;
3) bulk polymer that makes being used the volume ratio of methyl alcohol and glacial acetic acid is extract extracting 24h in apparatus,Soxhlet's of 9: 1, and vacuum-drying 10～12h under 60 ℃ of temperature condition promptly obtains the grand high selection adsorption functional material of chlorine sulphur then.
2. the preparation method of the grand molecularly imprinted polymer of a kind of chlorine sulphur according to claim 1; It is characterized in that: said N; The volume ratio of dinethylformamide and toluene is 0.5: 8, and chlorine sulphur is grand, the molar ratio of ionic liquid, ethylene glycol dimethacrylate is 1.5: 3.6: 8.
3. the preparation method of the grand molecularly imprinted polymer of a kind of chlorine sulphur according to claim 1, it is characterized in that: the extracting solution methyl alcohol of described methyl alcohol and glacial acetic acid and the volume ratio of glacial acetic acid are 9: 1.
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| CN2010102727224A CN102382248A (en) | 2010-09-06 | 2010-09-06 | Preparation method of chlorsulfuron molecular imprinting polymer |
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| CN2010102727224A CN102382248A (en) | 2010-09-06 | 2010-09-06 | Preparation method of chlorsulfuron molecular imprinting polymer |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102675506A (en) * | 2012-06-12 | 2012-09-19 | 福州大学 | 6-kinetin molecularly imprinted polymer and application thereof |
| CN105017482A (en) * | 2015-06-23 | 2015-11-04 | 嘉兴学院 | Surface molecularly imprinted poly(ionic liquid) for detecting 4-nonyl phenol and its preparation method and use |
| CN105498721A (en) * | 2015-11-23 | 2016-04-20 | 天津科技大学 | Aflatoxin molecularly imprinted material and preparation method thereof |
| CN105837747A (en) * | 2016-04-13 | 2016-08-10 | 河南师范大学 | Surface molecularly imprinted polymer used for selectively absorbing sulfamonomethoxine and preparation method thereof and application thereof |
| CN106046239A (en) * | 2016-07-29 | 2016-10-26 | 云南省烟草农业科学研究院 | Preparation method and application of chlorsulfuronmolecularly imprinted polymer |
| CN107383277A (en) * | 2017-07-28 | 2017-11-24 | 厦门大学 | Preparation using poly ion liquid as the sulfonylurea molecular engram material of function monomer |
-
2010
- 2010-09-06 CN CN2010102727224A patent/CN102382248A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102675506A (en) * | 2012-06-12 | 2012-09-19 | 福州大学 | 6-kinetin molecularly imprinted polymer and application thereof |
| CN102675506B (en) * | 2012-06-12 | 2013-12-11 | 福州大学 | 6-kinetin molecularly imprinted polymer and application thereof |
| CN105017482A (en) * | 2015-06-23 | 2015-11-04 | 嘉兴学院 | Surface molecularly imprinted poly(ionic liquid) for detecting 4-nonyl phenol and its preparation method and use |
| CN105017482B (en) * | 2015-06-23 | 2017-03-15 | 嘉兴学院 | For detecting surface molecule print poly ion liquid of 4 nonyl phenols and its production and use |
| CN105498721A (en) * | 2015-11-23 | 2016-04-20 | 天津科技大学 | Aflatoxin molecularly imprinted material and preparation method thereof |
| CN105498721B (en) * | 2015-11-23 | 2018-03-09 | 天津科技大学 | A kind of aflatoxin molecular engram material and preparation method thereof |
| CN105837747A (en) * | 2016-04-13 | 2016-08-10 | 河南师范大学 | Surface molecularly imprinted polymer used for selectively absorbing sulfamonomethoxine and preparation method thereof and application thereof |
| CN105837747B (en) * | 2016-04-13 | 2018-11-20 | 河南师范大学 | A kind of molecular imprinted polymer on surface and its preparation method and application for selective absorption daimeton |
| CN106046239A (en) * | 2016-07-29 | 2016-10-26 | 云南省烟草农业科学研究院 | Preparation method and application of chlorsulfuronmolecularly imprinted polymer |
| CN107383277A (en) * | 2017-07-28 | 2017-11-24 | 厦门大学 | Preparation using poly ion liquid as the sulfonylurea molecular engram material of function monomer |
| CN107383277B (en) * | 2017-07-28 | 2019-11-01 | 厦门大学 | Using poly ion liquid as the preparation of the sulfonylurea molecular engram material of function monomer |
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Application publication date: 20120321 |