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

Inactive Publication Date: 2015-01-14
LANZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006]Currently, most fluorescent imprinting materials use quantum dots or hybrid quantum dots as fluorescent sensing units. However, most of the prepared quantum dots have small core particle size and high surface energy, and the material is easy to agglomerat

Method used

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  • Preparation of core-shell ultraviolet fluorescence molecularly-imprinted material and application of material in sulfanilamide detection
  • Preparation of core-shell ultraviolet fluorescence molecularly-imprinted material and application of material in sulfanilamide detection
  • Preparation of core-shell ultraviolet fluorescence molecularly-imprinted material and application of material in sulfanilamide detection

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Experimental program
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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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Abstract

The invention relates to preparation of a core-shell ultraviolet fluorescence molecularly-imprinted material and application of the material in sulfanilamide detection. By using sulfamethyldiazine as a template molecule, the synthesized lysine-based fluorescence molecule as the functional monomer, ethylene glycol dimethyl acrylate as a crosslinking agent and azodiisobutyronitrile as an initiator, the lysine-framework fluorescence functional monomer with FMOC fluorophore is subjected to surface polymerization to obtain an about 10nm imprinted layer on the monodisperse methylacryloylated silicon ball surface with the diameter of 100nm. A Soxhlet method is utilized to remove the imprinted template molecule in the material to obtain the fluorescence molecularly-imprinted sensing material with fluorescence quenching responsiveness to the template molecule; the molecularly-imprinted material has the advantages of favorable dispersity, high response speed and stable optical properties, and is applicable to determining the sulfamethyldiazine content in the marked milk; and the method can indirectly convert the ultraviolet absorption signal of the analyte into a sensitive fluorescence signal, thereby enhancing the detection sensitivity and obtaining favorable recovery rate.

Description

technical field [0001] The invention relates to a preparation method of a core-shell fluorescent molecularly imprinted polymer functionalized with ultraviolet fluorescent groups, and belongs to the technical field of preparation of functional nanometer materials. [0002] Background technique [0003] The antibiotic residues caused by the abuse of antibiotics are undoubtedly the "accelerated evolution" of the resistance of pathogenic bacteria, and "drug-resistant bacteria" are largely caused by the abuse of antibiotics. If this situation continues to spread and worsen, it is likely that humans will face a situation where there is no medicine available for infection. At present, a variety of instrumental analysis methods have been established for the detection of antibiotic residues in food, but all of them must rely on sophisticated and expensive instruments, which are time-consuming and laborious to operate and process, and are not suitable for on-site and rapid analysis. ...

Claims

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Application Information

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IPC IPC(8): C08F292/00C08F222/38C08F222/14B01J20/26B01J20/30G01N21/64
Inventor 张海霞于辨非张健健杨艳杰张柯林
Owner LANZHOU UNIVERSITY
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