Method for detecting ofloxacin in milk by combination of magnetic solid-phase microextraction and carbon quantum dot fluorescence sensibilization

A technology of carbon quantum dots and ofloxacin, applied in the field of magnetic solid-phase microextraction combined with carbon quantum dots fluorescence sensitization detection of ofloxacin in milk, to achieve fast separation speed, good specificity, and fast magnetic separation speed Effect

Active Publication Date: 2018-02-13
KUNMING UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In recent years, there are a lot of bibliographical reports about nitrogen-doped carbon quantum dots, and the fluorescence quantum yield of carbon quantum dots has been improved, and there is no report identical with the method of the present invention

Method used

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  • Method for detecting ofloxacin in milk by combination of magnetic solid-phase microextraction and carbon quantum dot fluorescence sensibilization
  • Method for detecting ofloxacin in milk by combination of magnetic solid-phase microextraction and carbon quantum dot fluorescence sensibilization
  • Method for detecting ofloxacin in milk by combination of magnetic solid-phase microextraction and carbon quantum dot fluorescence sensibilization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1: the assay steps of ofloxacin in milk are as follows:

[0028] (1) Preparation of water-soluble nitrogen-doped fluorescent carbon quantum dots (N-CQDs): Weigh 10.0 g of polyethyleneimine liquid, add it to 90 mL of ultrapure water, and ultrasonically mix it thoroughly for 5 minutes, and transfer it to a polymer Tetrafluoroethylene reaction kettle, heated at 200°C for 5 hours, cooled naturally to room temperature, first filtered with a filter membrane with a pore size of 0.22 μm, and then dialyzed with a dialysis bag with a molecular weight cut-off of 3500Da for 24 hours to obtain water-soluble nitrogen-doped fluorescence carbon quantum dots;

[0029] (2) The preparation methods of magnetic nanomaterials include:

[0030] Fe 3 o 4 Preparation: Take 2.05g of ferrous ammonium sulfate and 1.41g of ferric chloride, dissolve them in 50mL of deionized water, and heat them in a water bath to 80°C under the protection of nitrogen, add 5mL of ammonia water with a...

Embodiment 2

[0037] Embodiment 2: the assay steps of ofloxacin in milk are as follows:

[0038] (1) Preparation of water-soluble nitrogen-doped fluorescent carbon quantum dots: Weigh 12.0 g of polyethyleneimine liquid, add it to 90 mL of ultrapure water, ultrasonically mix it thoroughly for 10 min, and transfer it to a polytetrafluoroethylene reactor , heated at 250°C for 6 hours, cooled to room temperature naturally, filtered with a filter membrane with a pore size of 0.22 μm, and then dialyzed with a dialysis bag with a molecular weight cut-off of 3000 Da for 24 hours to obtain water-soluble nitrogen-doped fluorescent carbon quantum dots;

[0039] (2) The preparation methods of magnetic nanomaterials include:

[0040] Fe 3 o 4 Preparation: Take 2.20g of ferrous ammonium sulfate and 1.65g of ferric chloride, dissolve them in 50mL of deionized water, and heat them in a water bath to 75°C under nitrogen protection, then add 6mL of ammonia water with a concentration of 28% by volume and ...

Embodiment 3

[0046] Embodiment 3: the assay steps of ofloxacin in milk are as follows:

[0047] (1) Weigh 15.0g of polyethyleneimine liquid, add it to 90mL of ultrapure water, mix it thoroughly by ultrasonication for 8min, transfer it to a polytetrafluoroethylene reactor, heat at 220°C for 10h, and cool down to room temperature naturally , first filter with a filter membrane with a pore size of 0.22 μm, and then perform dialysis treatment with a dialysis bag with a molecular weight cut-off of 3200 Da for 24 hours to obtain water-soluble nitrogen-doped fluorescent carbon quantum dots;

[0048] (2) The preparation methods of magnetic nanomaterials include:

[0049] Fe 3 o 4 Preparation: Take 2.50g of ferrous ammonium sulfate and 2.00g of ferric chloride, dissolve them in 50mL of deionized water, and heat them in a water bath to 85°C under the protection of nitrogen, add 7mL of ammonia water with a concentration of 28% by volume, and continue stirring React for 30 minutes, cool to room t...

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Abstract

The invention discloses a method for detecting ofloxacin in milk by combination of magnetic solid-phase microextraction and carbon quantum dot fluorescence sensibilization. According to the method, polyethylenimine is utilized as a carbon source and a nitrogen source, and nitrogen doped fluorescent carbon quantum dots are synthesized by a hydrothermal method; ferroferric oxide magnetic nano particles modified by 2-(5-bromine-pyridine azo)-5-diethylamino phenol and lauryl sodium sulfate are utilized as a milk purifying material, the ofloxacin can enhance fluorescence of the nitrogen doped fluorescent carbon quantum dots, the strength of a fluorescent signal enhanced by the ofloxacin and the concentration of the ofloxacin have a certain linear relation, and a fluorescence spectrophotometry for detecting the ofloxacin can be established based on the certain linear relation. The nitrogen doped fluorescent carbon quantum dots prepared by the method disclosed by the invention have a remarkable fluorescence sensibilization effect and strong selectivity; the magnetic nano particles have a better purifying effect and can eliminate matrix interference; the method can be applied to fluorescence measurement of the ofloxacin and has the characteristics of high flexibility and specificity.

Description

technical field [0001] The invention relates to the technical field of chemical analysis and detection, in particular to a method for detecting ofloxacin in milk in combination with magnetic solid-phase microextraction and carbon quantum dot fluorescence sensitization. Background technique [0002] Ofloxacin is a synthetic quinolone broad-spectrum antibiotic widely used in the dairy industry to treat mastitis in dairy cows. Its residues pose serious threats to human health, such as allergic reactions and drug-resistant bacteria in the body. Therefore, my country and some other countries have established strict control standards for the residues of antibiotics such as ofloxacin in dairy products. Traditional methods for the determination of antibiotic residues, such as ELISA, chromatography, etc., require complex sample pretreatment of the milk matrix. The fluorescence method has the characteristics of simple operation, rapidity, and high sensitivity, but the interference ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64C09K11/65B82Y20/00B82Y40/00
CPCB82Y20/00B82Y40/00C09K11/0883C09K11/65G01N21/6428G01N2021/6432
Inventor 杨亚玲华建豪杨德志
Owner KUNMING UNIV OF SCI & TECH
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