Preparation of a core-shell UV fluorescent molecularly imprinted material and its application in the detection of sulfonamide

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: 2016-08-24
LANZHOU UNIVERSITY
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0005] At present, most fluorescent imprinting materials use quantum dots or hybrid quantum dots as fluorescent sensing units. Most of the preparation processes are cumbersome, and due to the size limitation of quantum effects, most of the prepared quantum dots have a small core particle size and a large surface area. High energy, the material is easy to agglomerate when modifying the imprinted layer, which affects the dispersion and optical stability of the final imprinted material ( RSCAdv., 2014, 4, 2764–2771 ) ( Biosensors and Bioelectronics 2014, 57, 310–316 ), and then Affect the reproducibility of test results

Method used

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  • Preparation of a core-shell UV fluorescent molecularly imprinted material and its application in the detection of sulfonamide
  • Preparation of a core-shell UV fluorescent molecularly imprinted material and its application in the detection of sulfonamide
  • Preparation of a core-shell UV fluorescent molecularly imprinted material and its application in the detection of sulfonamide

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Embodiment 1

[0034] Preparation of fluorescent functional monomer: Add 2.5 g of N-fluorenylmethylformyl-N-tert-butylformyl-lysine (FMOC-Lys-BOC) into 40 ml of methanol saturated with hydrogen chloride gas, and stir at room temperature for 2 After 1 hour, it was suction filtered, washed 3 times with 25 ml of methanol, and dried to obtain FMOC-protected lysine methyl ester hydrochloride. Take 3 mmol of the raw material that has completely removed BOC and add it to 25 ml of anhydrous dichloromethane (DCM). After adding 3.3 mmol of methacryloyl chloride, add 6 mmol of anhydrous triethylamine (TEA) dropwise. After 1 hour of reaction, add 25 ml of Diluted in dichloromethane (DCM), then washed successively with hydrochloric acid with pH = 1 and saturated brine, the organic phase was dried over anhydrous sodium sulfate, concentrated and purified by column (ethyl acetate: petroleum ether = 1:2), The product was spin-dried to obtain white crystals of N-fluorenylmethylformyl-N-methacryloyl-lysine met...

Embodiment 2

[0040] Five batches of fluorescent imprinted materials doped with different functional monomers were prepared by bulk polymerization (from which the optimal raw material ratio was screened out): Taking the fluorescent imprinted materials doped with methacrylic acid (MAA) functional monomer as an example, 0.15 Add 1 mmol template molecule SMZ and 0.45 mmol MAA to a 3 ml vial with a cap, then add 1.5 ml N,N-dimethylformamide (DMF) to dissolve, stir magnetically for 1 h, then add fluorescent monomer FMOC-Lys-MC , stirred at room temperature for 1 hour after bubbling nitrogen gas, and left overnight. Then add 1.5 mmol of cross-linking agent ethylene glycol dimethacrylate (EGDMA) and 6 mg of initiator azobisisobutyronitrile (AIBN) in sequence, stir at 60°C for 20 hours after nitrogen blowing, grind and sieve, then Soxhlet wash (methanol: acetic acid = 8:1) until the supernatant has no UV absorption of template molecules, dry it under vacuum at 60°C for use. This material number is...

Embodiment 3

[0042] Preparation of methacrylic silicon sphere carrier: mix 80 ml of ethanol, 6 ml of water, and 3 ml of ammonia water, add 8 ml of tetraethyl orthosilicate (TEOS) dropwise under stirring, react at room temperature for 8 hours, and centrifuge with ethanol Wash twice, then disperse the resulting silicon spheres into 60 ml of ethanol, add 0.5 ml of water and 0.1 ml of ammonia water, add 1 ml of methacrylpropyltrimethoxysilane (MPS) dropwise under stirring, and react for 12 hours Centrifuge and wash with ethanol for 3 times, and vacuum-dry at 50°C to obtain 2.28 g of methacrylylated silicon spheres, which are refrigerated for use.

[0043] Add 0.15 mmol of the template molecule SMZ and 0.15 mmol of the fluorescent monomer FMOC-Lys-MC into 25 ml of acetonitrile for ultrasonic dissolution, and stir at room temperature for 5 hours after bubbling with nitrogen, then add 1.5 mmol of cross-linking agent EGDMA and 300 mg of methacryl 5 ml of acetonitrile solution of silicon spheres, 0...

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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. Background technique [0002] 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. Therefore,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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