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Preparation method of electrochemical sensor for detection of sulfonamide veterinary drug residues

A veterinary drug residue and electrochemical technology, applied in the direction of material electrochemical variables, can solve the problems of high detection cost, complex analysis procedures, long detection cycle, etc., and achieve fast response, high sensitivity, and good repeatability

Active Publication Date: 2017-09-26
HENAN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the analytical methods for the determination of sulfa drugs in various biological matrices mainly include high performance liquid chromatography (HPLC), liquid chromatography-tandem mass spectrometry (LC-MS-MS), capillary electrophoresis-mass spectrometry (CE-MS), etc. Although these methods have the advantages of high sensitivity and accuracy and can measure multiple components at one time, they require large and expensive instruments and complex sample purification and preparation procedures. The analysis procedures are complicated, the detection period is long, and the detection cost is high. Moreover, the detection technology level is relatively high, and professional technicians are needed to complete it. It is difficult to popularize it in grassroots units, and it is difficult to comprehensively monitor the breeding, processing, and circulation of poultry, livestock, and fish.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Specific steps are as follows:

[0017] (1) The multi-walled carbon nanotube raw material was purified and oxidized by the mixed acid liquid phase oxidation method, and 0.5 g of the multi-walled carbon nanotube was weighed and added to 20 mL of the mixed acid solution (concentrated HNO 3 with concentrated H 2 SO 4 The volume ratio is 1:2), ultrasonic oxidation and dispersion for 2h. The mixture was vacuum filtered through polycarbonate filter paper with a pore size of 0.02 μm, and then washed with deionized water until the pH value was 7, and the treated multi-walled carbon nanotubes were vacuum-dried at 80 °C for 2 h. Use Nafion to compound and functionalize multi-walled carbon nanotubes by surface deposition cross-linking method, weigh 100 mg of the above-mentioned purified and oxidized multi-walled carbon nanotubes and dissolve them in a 3% Nafion solution with a pH value of 7.0 phosphate In the mixed solution of the buffer solution (the volume ratio of Nafion sol...

Embodiment 2

[0021] Specific steps are as follows:

[0022] (1) The mixed acid liquid phase oxidation method was used to purify and oxidize the raw materials of multi-walled carbon nanotubes. Weighed 0.8g multi-walled carbon nanotubes and added them to 40mL mixed acid solution (concentrated HNO 3 with concentrated H 2 SO 4 The volume ratio is 1:3), ultrasonic oxidation and dispersion for 3h. The mixture was vacuum filtered through a polycarbonate filter paper with a pore size of 0.04 μm, and then washed with deionized water until the pH value was 7, and the treated multi-walled carbon nanotubes were vacuum-dried at 90 °C for 3 h. The multi-walled carbon nanotubes were compounded and functionalized by Nafion by surface deposition and cross-linking method, and 200 mg of the above-mentioned purified and oxidized multi-walled carbon nanotubes were weighed and dissolved in a 5% Nafion solution and a pH value of 7.0 phosphate buffer In the mixed solution of Nafion solution and phosphate buffe...

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Abstract

The invention relates to a preparation method of an electrochemical sensor for the detection of sulfonamide veterinary drug residues, comprising the following steps: using mixed acid oxidation treated multi-walled carbon nanotubes as filling materials, using Nafion solution as the dispersion of multi-walled carbon nanotubes Reagent, using hydroxycarboxyl reactant as cross-linking agent to obtain Nafion-multi-walled carbon nanotube functionalized nanomaterials; use platinum wire and soft glass tube to obtain platinum microelectrode, after chemical corrosion, take appropriate amount of Nafion-multi-walled carbon Nanotube functionalized nanomaterials are prepared by grinding, pressing and filling method to prepare embedded Nafion-multi-walled carbon nanotube micro-electrodes. Meanwhile, the present invention simplifies three electrodes into a two-electrode system, and uses embedded Nafion-multi-walled carbon nanotube micro-electrodes as the work The electrode is used as the reference electrode and the counter electrode, and an electrochemical sensor for the detection of sulfonamide veterinary drug residues is obtained. Compared with the traditional macro electrode glassy carbon electrode, the invention has the advantages of fast response speed, high signal-to-noise ratio, high sensitivity, good repeatability and high accuracy.

Description

technical field [0001] The invention relates to a method for preparing an electrochemical sensor for detecting residues of sulfonamide veterinary drugs, in particular to a method for preparing a novel microelectrode based on embedded Nafion-multi-walled carbon nanotubes. Background technique [0002] Food is the most basic material condition for the survival and development of human society. The state of food safety is directly related to the health and life safety of the broad masses of the people, and is related to the coordinated development of my country's national economy and society. "Prominent source pollution" is a potential threat to my country's food safety. In the breeding industry, in order to prevent and treat diseases of livestock, poultry, fish, etc., a large amount of drugs such as antibiotics, sulfonamides, hormones, etc. have been invested, resulting in drug residues in animal foods. , Application before slaughter, drug residues are more serious. Veterina...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/30
Inventor 何保山谢岩黎卫敏赵文红陈文博张俊霞
Owner HENAN UNIVERSITY OF TECHNOLOGY
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