Preparation of core-shell ultraviolet fluorescence molecularly-imprinted material and application of material in sulfanilamide detection
A fluorescent molecular imprinting and ultraviolet technology, which is applied in the direction of fluorescence/phosphorescence, material excitation analysis, and other chemical processes, can solve the problems affecting the dispersion and optical stability of imprinted materials, the reproducibility of detection results, and the particle size of the quantum dot core. Small and other problems, to achieve the effect of uniform shape, stable optical properties, and easy preparation
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Embodiment 1
[0035] Preparation of fluorescent functional monomer: add 2.5g of N-fluorenyl methyl formyl-N-tert-butyl formyl-lysine (FMOC-Lys-BOC) to 40 ml methanol saturated with hydrogen chloride gas, and stir at room temperature for 2 After hours, it was filtered with suction, washed with 25 ml methanol 3 times, and dried to obtain FMOC-protected lysine methyl ester hydrochloride. Take 3 mmol of the raw material from which BOC has been removed and add it to 25ml of anhydrous dichloromethane (DCM), add 3.3 mmol of methacryloyl chloride, and then add 6 mmol of anhydrous triethylamine (TEA) dropwise. The reaction is completed for 1 hour, and 25ml is added. Dilute in water with dichloromethane (DCM), then wash with pH=1 hydrochloric acid and saturated brine in turn, the organic phase is dried with anhydrous sodium sulfate and concentrated on a column for purification (ethyl acetate: petroleum ether=1:2), The product was spin-dried to obtain white crystals of N-fluorene methyl formyl-N-methac...
Embodiment 2
[0041] Five batches of fluorescent imprinting materials doped with different functional monomers were prepared by bulk polymerization (the optimal raw material ratio was selected from them): Take the fluorescent imprinting materials doped with methacrylic acid (MAA) functional monomers as an example, and 0.15 Add mmol template molecule SMZ and 0.45 mmol MAA into a 3 ml vial with lid, then add 1.5 ml N,N-dimethylformamide (DMF) to dissolve, magnetically stir for 1 h, then add fluorescent monomer FMOC-Lys-MC After bubbling nitrogen, stir at room temperature for 1 hour, and let stand overnight. Then add 1.5 mmol crosslinker ethylene glycol dimethacrylate (EGDMA) and 6 mg initiator azobisisobutyronitrile (AIBN) in sequence, bubbling with nitrogen and stirring at 60°C for 20 hours, grinding and sieving, and Soxhlet washing (Methanol: acetic acid=8:1) until the supernatant has no ultraviolet absorption of the template molecules, vacuum dry at 60°C for later use. The material number ...
Embodiment 3
[0043] Preparation of methacrylylated silica ball carrier: After mixing 80 ml of ethanol, 6 ml of water, and 3 ml of ammonia water, add 8 ml of tetraethyl orthosilicate (TEOS) dropwise with stirring, react at room temperature for 8 hours and then centrifuge with ethanol Wash twice, then disperse the obtained silicon balls into 60 ml ethanol, add 0.5 ml water and 0.1 ml ammonia water, add 1 ml methacryloylpropyltrimethoxysilane (MPS) dropwise with stirring, and react for 12 hours It was centrifuged and washed with ethanol three times, and dried under vacuum at 50° C. to obtain 2.28 g of methacryloyl silica balls, which were refrigerated for use.
[0044] Add 0.15 mmol template molecule SMZ and 0.15 mmol fluorescent monomer FMOC-Lys-MC to 25ml acetonitrile to dissolve ultrasonically, bubbling nitrogen gas and stirring at room temperature for 5 hours, then add 1.5 mmol crosslinker EGDMA and 300 mg methacrylic acid in turn 5 ml of acetonitrile solution of silicon balls, 0.06 mmol of ...
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