CN103275271A - Preparation method of chloramphenicol molecularly-imprinted polymer film - Google Patents
Preparation method of chloramphenicol molecularly-imprinted polymer film Download PDFInfo
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- CN103275271A CN103275271A CN2013101513698A CN201310151369A CN103275271A CN 103275271 A CN103275271 A CN 103275271A CN 2013101513698 A CN2013101513698 A CN 2013101513698A CN 201310151369 A CN201310151369 A CN 201310151369A CN 103275271 A CN103275271 A CN 103275271A
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Abstract
The invention discloses a preparation method of a chloramphenicol molecularly-imprinted polymer film. The preparation method comprises the following steps of 1, dissolving chloramphenicol as a template molecule, N,N-diethylaminoethyl methacrylate as a functional monomer and ethylene glycol dimethacrylate as a cross-linking agent in tetrahydrofuran as a pore forming agent according to a mole ratio of 1: 4: 20, and carrying out ultrasonic treatment for 30min, wherein a use amount ratio of tetrahydrofuran to chloramphenicol is 5ml/0.25mmol, 2, adding azodiisobutyronitrile as an initiator into the mixed solution, and carrying out ultrasonic treatment for 15min, wherein a use amount ratio of azodiisobutyronitrile to chloramphenicol is 10mg/0.25mmol, 3, immersing a film carrier into the solution obtained by the step 2 for 20min, extruding the immersed film carrier until bubbles disappear, putting the film carrier into a sealing bag, filling nitrogen into the sealing bag, carrying out sealing, and carrying out ultraviolet lamp irradiation to initiate polymerization lasting for 12h, and 4, putting the film carrier into a methanol-acetic acid mixed solution, wherein a volume ratio of methanol to acetic acid is 3: 1, and carrying out ultrasonic elution for 24h to obtain the chloramphenicol molecularly-imprinted polymer film.
Description
Technical field
The present invention relates to a kind of preparation method of molecular imprinted polymer membrane, especially a kind of preparation method of the chloramphenicol molecularly imprinted polymeric film to paraxin highly selective absorption.
Background technology
(Chloramphenicol is nineteen forty-seven to separate the microbiotic that obtains first from microbe metabolite CAP) to paraxin, owing to its good germ resistance, the stable property of medicine, cheap price, extensively as fodder additives, is used for the treatment of bacteriosis.Yet owing to be with nitro on its phenyl ring, its half life of decomposition is long and have serious toxic side effect, easily causes the human body blood poisoning, causes serious toxic side effect such as irreversible aplastic anemia, and human beings'health is constituted huge potential threat.Therefore, European Union, the U.S. all in rules the residual limit standard of regulation CAP be " zero tolerance ", China Ministry of Agriculture also regulation CAP and salt, fat etc. must not detect in all edible tissues of food animal.At present, mainly contain microbial method, immunoassay, vapor-phase chromatography, combined gas chromatography mass spectrometry, supercritical fluid chromatography and immunofluorescence capillary electrophoresis technique etc. for CAP detection method residual in the sample.Existing detection method is for the sample pre-treatments complex steps, and sample matrix complicated component, CAP residual concentration are low in addition, are difficult to realize effectively detecting fast.Its ultimate principle of molecular imprinting (molecular imprinting technology MIT) is that template molecule is (to be separated, the molecule of identification) interacts with the function monomer with suitable functional group, under linking agent and action of evocating, form and have macropore, netted polymkeric substance, remove template molecule by solvent elution or hydrolysis under certain condition, just stayed size in the polymkeric substance, " memory " hole of shape and functional group and template molecule coupling, specific affinity interaction just can be carried out with template molecule to be separated in the mixture in such hole, thereby reach separation, purifying, pre-concentration template molecule etc., then with chemiluminescence methods such as enzyme linked immunologicals, can realize to template molecule in the sample fast, effectively detect.But, up to now also not about preparing the relevant report of chloramphenicol molecularly imprinted polymeric film.
Summary of the invention
The present invention is in order to solve the above-mentioned technical problem of existing in prior technology, and a kind of preparation method of the chloramphenicol molecularly imprinted polymeric film to the absorption of paraxin highly selective is provided.
Technical solution of the present invention is: a kind of preparation method of chloramphenicol molecularly imprinted polymeric film is characterized in that carrying out as follows successively:
A. template molecule paraxin, function monomer diethyl aminoethyl methacrylate and linking agent ethylene glycol dimethacrylate are dissolved in the pore-creating agent tetrahydrofuran (THF) ultrasonic 30min according to mol ratio 1:4:20; The consumption of described tetrahydrofuran (THF) is 5ml/0.25mmol paraxin;
B. add the initiator Diisopropyl azodicarboxylate, ultrasonic 15min, add-on is 10mg/0.25mmol paraxin;
C. membrane carrier is immersed 20min in the b step gained solution, push membrane carrier after the immersion liquid again to there not being bubble, put into sealing bag, charge into nitrogen, under sealing and the ultra violet lamp condition, initiated polymerization 12h;
D. membrane carrier being placed volume ratio is methyl alcohol-acetic acid mixed solution of 3:1 again, and ultrasonic wash-out 24 hours obtains the chloramphenicol molecularly imprinted polymeric film.
Described membrane carrier is nylon membrane, polypropylene screen or polyvinylidene fluoride film.
Described a step is to take by weighing 0.25mmol paraxin in flask, to wherein adding the 5ml tetrahydrofuran (THF), ultrasonic 5min; After treating the paraxin dissolving, add people 1mmol diethyl aminoethyl methacrylate, ultrasonic 20min; Again the 5.0mmol ethylene glycol dimethacrylate is joined in the flask ultrasonic 5min.
The present invention is to be function monomer with the diethyl aminoethyl methacrylate, be that linking agent, tetrahydrofuran (THF) are that pore-creating agent, Diisopropyl azodicarboxylate are initiator with the ethylene glycol dimethacrylate, and according to specified proportion and working condition etc., produce and have very high selectivity and specific chloramphenicol molecularly imprinted polymeric film, advantages of higher stability, long work-ing life and stronger anti-adverse environment ability are arranged.The present invention is with low cost, simple to operate, easy control of reaction conditions.
Description of drawings
Fig. 1 is that the embodiment of the invention is to the paraxin methanol solution adsorptive power synoptic diagram of different concns.
Fig. 2 is that the embodiment of the invention is to the paraxin methanol solution curve of adsorption kinetics of 50mg/L concentration.
Embodiment
A. take by weighing 0.25mmol paraxin in flask, to wherein adding the 5ml tetrahydrofuran (THF), ultrasonic 5min; After treating the paraxin dissolving, add people 1mmol diethyl aminoethyl methacrylate, ultrasonic 20min; Again the 5.0mmol ethylene glycol dimethacrylate is joined in the flask ultrasonic 5min;
B. add 10mg initiator Diisopropyl azodicarboxylate, ultrasonic 15min;
C. membrane carriers such as nylon membrane, polypropylene screen or polyvinylidene fluoride film are immersed 20min in the b step gained solution, membrane carrier after will having soaked with two blocks of sheet glass is again clamped, and being squeezed to does not have bubble, puts into sealing bag, charge into nitrogen, ultra violet lamp (the initiated polymerization 12h of λ=365nm);
D. membrane carrier being placed volume ratio is methyl alcohol-acetic acid mixed solution of 3:1 again, and ultrasonic wash-out 24 hours changed elutriant one time in per six hours, removed template molecule, obtained the chloramphenicol molecularly imprinted polymeric film.
The absorption property test:
Paraxin-the methanol solution of a series of change in concentration of 10 ml (10 ~ 120 mg/L) is placed 25 ml tool plug Erlenmeyer flasks respectively, respectively to the blotting membrane of wherein putting into a slice embodiment of the invention and non-blotting membrane, place it on the micro oscillator room temperature 2 h that vibrate, after finishing, vibration leaves standstill 10 min, get an amount of supernatant liquor and be diluted to certain volume with methyl alcohol, measure the absorbancy of paraxin in the equilibrium adsorption solution with ultraviolet spectrophotometer.The result as shown in Figure 1.
Fig. 1 has showed the paraxin blotting membrane (CAP) of the embodiment of the invention and non-blotting membrane (NCAP) to the adsorptive power of the paraxin methanol solution (10-120 mg/L) of a series of concentration, and the adsorptive power of embodiment of the invention blotting membrane is better than non-blotting membrane and both adsorptive poweies all raise along with the rising of paraxin initial concentration as can be seen.Be under 120 mg/L in concentration, embodiment of the invention blotting membrane reaches maximal absorptive capacity 8.624 μ g/ films, is 3.152 μ g/ films with the non-blotting membrane adsorptive capacity under the concentration, and the adsorptive capacity of blotting membrane has surpassed 5.0 times of non-blotting membrane under this concentration.
Because curve of adsorption kinetics do not change with the change of substrate initial concentration, and the paraxin adsorptive capacity has rapid trend of rising in concentration during for 50mg/L, therefore is chosen under this concentration and draws curve of adsorption kinetics, as shown in Figure 2.
As shown in Figure 2, embodiment of the invention blotting membrane rate of adsorption is fast, has adsorbed 70% of maximum in the time of 25 minutes, and reaches adsorption equilibrium substantially in the time of 50 minutes.
Claims (3)
1. the preparation method of a chloramphenicol molecularly imprinted polymeric film is characterized in that carrying out as follows successively:
A. template molecule paraxin, function monomer diethyl aminoethyl methacrylate and linking agent ethylene glycol dimethacrylate are dissolved in the pore-creating agent tetrahydrofuran (THF) ultrasonic 30min according to mol ratio 1:4:20; The consumption of described tetrahydrofuran (THF) is 5ml/0.25mmol paraxin;
B. add the initiator Diisopropyl azodicarboxylate, ultrasonic 15min, add-on is 10mg/0.25mmol paraxin;
C. membrane carrier is immersed 20min in the b step gained solution, push membrane carrier after the immersion liquid again to there not being bubble, put into sealing bag, charge into nitrogen, under sealing and the ultra violet lamp condition, initiated polymerization 12h;
D. membrane carrier being placed volume ratio is methyl alcohol-acetic acid mixed solution of 3:1 again, and ultrasonic wash-out 24 hours obtains the chloramphenicol molecularly imprinted polymeric film.
2. according to the preparation method of the described chloramphenicol molecularly imprinted polymeric film of claim 1, it is characterized in that: described membrane carrier is nylon membrane, polypropylene screen or polyvinylidene fluoride film.
3. the preparation method of chloramphenicol molecularly imprinted polymeric film according to claim 1 and 2, it is characterized in that: described a step is to take by weighing 0.25mmol paraxin in flask, to wherein adding the 5ml tetrahydrofuran (THF), ultrasonic 5min; After treating the paraxin dissolving, add people 1mmol diethyl aminoethyl methacrylate, ultrasonic 20min; Again the 5.0mmol ethylene glycol dimethacrylate is joined in the flask ultrasonic 5min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103497350A (en) * | 2013-09-12 | 2014-01-08 | 西安交通大学 | Preparation method of cloxacillin molecular imprinting polymer membrane |
| CN103497277A (en) * | 2013-09-09 | 2014-01-08 | 南京医科大学 | Baicalein molecularly imprinted polymer, preparation method 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 |
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| CN101387617A (en) * | 2008-10-16 | 2009-03-18 | 上海交通大学 | Silk-screen printing electrode and method for synthesizing chloramphenicol molecular imprinting film |
| CN102617788A (en) * | 2012-03-29 | 2012-08-01 | 常熟市海虞茶叶有限公司 | Salinomycin molecularly imprinted polymer and preparation method thereof |
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| CN101387617A (en) * | 2008-10-16 | 2009-03-18 | 上海交通大学 | Silk-screen printing electrode and method for synthesizing chloramphenicol molecular imprinting film |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103497277A (en) * | 2013-09-09 | 2014-01-08 | 南京医科大学 | Baicalein molecularly imprinted polymer, preparation method and application thereof |
| CN103497277B (en) * | 2013-09-09 | 2016-04-27 | 南京医科大学 | Scutellarin molecularly imprinted polymer and its preparation method and application |
| CN103497350A (en) * | 2013-09-12 | 2014-01-08 | 西安交通大学 | Preparation method of cloxacillin molecular imprinting polymer membrane |
| CN103497350B (en) * | 2013-09-12 | 2015-07-01 | 西安交通大学 | Preparation method of cloxacillin molecular imprinting polymer membrane |
| 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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Application publication date: 20130904 |