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Thermal polymerization preparation method of tetracycline molecular imprinted polymer membrane electrode

A polymer film and molecular imprinting technology, which is applied in the analysis of materials, material analysis by electromagnetic means, and measurement devices, can solve the problems of low detection sensitivity, need for large instruments, weak anti-interference performance, etc., and achieve high sensitivity and detection The effect of low limit value

Inactive Publication Date: 2010-03-17
DALIAN UNIV OF TECH
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  • Claims
  • Application Information

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Problems solved by technology

Tetracycline is one of the tetracycline antibiotics, and it has residues in many media such as milk and fish. At present, the commonly used detection methods mainly include microbial method, enzyme-linked immunosorbent assay, high performance liquid chromatography and liquid chromatography-tandem mass spectrometry etc. Some of these methods have low detection sensitivity, some have high cost or weak anti-interference performance, the pretreatment process is complicated, and large-scale instruments are required, which are not suitable for on-site and rapid detection.
Chinese patent application "Tetracycline Molecularly Imprinted Polymer Membrane Electrode and Its Preparation and Application" (Application No.: 200810012433.3) discloses a method for preparing a tetracycline molecularly imprinted polymer membrane electrode by photopolymerization, which is characterized in that: the template molecule hydrochloric acid Tetracycline, functional monomer styrene, cross-linking agent ethylene glycol dimethacrylate, initiator azobisisobutyronitrile, porogen methanol or chloroform or toluene are mixed and ultrasonically dissolved, and then polymerized on the electrode substrate by ultraviolet light Polymerization, but using this method, the tetracycline molecularly imprinted polymer film does not cover the surface of the electrode substrate uniformly, which will affect the sensitivity of tetracycline electrochemical detection

Method used

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  • Thermal polymerization preparation method of tetracycline molecular imprinted polymer membrane electrode

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Experimental program
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Effect test

Embodiment 1

[0021] Example 1, a tetracycline molecularly imprinted polymer membrane electrode was prepared by a thermal polymerization method using a platinum electrode as an electrode substrate.

[0022] Take 0.1g of tetracycline, 0.038mL of methacrylic acid, 3.53mL of ethylene glycol dimethacrylate (molar ratio 1:2:90), 0.05g of azobisisobutyronitrile, and 10mL of methanol. Ultrasonic dissolution is carried out in the washing machine to form a uniform sol-like compound.

[0023] Al 2 o 3 After the powder is ground, it is ultrasonically cleaned with ethanol and water respectively, and dried in the air.

[0024] Immerse the electrode in the above-prepared sol for 5 seconds, then place it in a sealable plastic tube, fill the tube with nitrogen to remove oxygen for 5 minutes, seal it and place it in a constant temperature water bath at 55°C, and polymerize for 12 hours; repeat Do this step once.

[0025] After two thermal polymerization reactions, the electrode was first soaked in ethan...

Embodiment 2

[0026] Example 2, a tetracycline molecularly imprinted polymer membrane electrode was prepared by thermal polymerization using a gold-deposited titanium electrode as the electrode substrate.

[0027] Take tetracycline 0.3g, methacrylic acid 0.305mL, ethylene glycol dimethacrylate 3.53mL (molar ratio is 3:15:90), azobisisobutyronitrile 0.06g, and 15mL chloroform after mixing, place in Ultrasonic dissolution is carried out in an ultrasonic cleaner to form a uniform sol-like compound.

[0028] The commercially pure titanium sheet (purity > 99%) with a size of 20mm×30mm was polished with 350#, 800#, 1000# and 1200# emery paper in sequence, then ultrasonically cleaned in ethanol solution for 3 minutes, and then deionized water Ultrasonic cleaning for 20 minutes to thoroughly clean the titanium sheet. Adopt three-electrode system to electrodeposit gold, deposition solution is 2g / L chloroauric acid solution, this chloroauric acid solution contains the hydrochloric acid solution of 0...

Embodiment 3

[0030] Example 3, a tetracycline molecularly imprinted polymer film electrode was prepared by thermal polymerization using a platinum-deposited titanium electrode as an electrode substrate and its application in electrochemical detection.

[0031] Take 0.2g of tetracycline, 0.135mL of methacrylic acid, 3.53mL of ethylene glycol dimethacrylate (the molar ratio is 2:7:90), 0.06g of azobisisobutyronitrile, and 14mL of methanol. Ultrasonic dissolution is carried out in the washing machine to form a uniform sol-like compound.

[0032] After the commercially pure titanium sheet (purity > 99%) with a size of 20mm * 30mm is polished and cleaned according to the process described in Example 2, platinum is electrodeposited using a three-electrode system, and the deposition solution is 2g / L chloroplatinic acid solution. The platinum acid solution contains 0.01 mmol / L hydrochloric acid solution, the deposition voltage is -0.35 V (relative to a saturated calomel electrode), and the deposit...

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Abstract

The invention relates to tetracycline molecular imprinted polymer and a method for preparing tetracycline molecular imprinted polymer membrane electrode. The method comprises the steps of: ultrasonicdissolving template molecule tetracycline, functional monomer methacrylic acid, crosslinker ethylene glycol dimethacrylate, initiator azodiisobutyronitrile, and cavity-inducing agent methanol or chloroform or toluol to form even sol compound; and under the condition of constant temperature at 55-65 DEG C, forming the tetracycline molecular imprinted polymer membrane electrode on the surface of electrode matrix by means of thermal polymerization and elution template molecule. The tetracycline molecular imprinted polymer membrane electrode can be taken as a work electrode for detecting the tetracycline in water body with the electrochemistry method, and is convenient for fasting detecting on the spot, wherein the detection range is 0.1-10mg / l, and the detection limit is 0.026mg / l.

Description

technical field [0001] The invention relates to a tetracycline molecularly imprinted polymer and a method for preparing a tetracycline molecularly imprinted polymer membrane electrode. Background technique [0002] Tetracycline antibiotics are a class of broad-spectrum antibiotics that are widely used in aquaculture and animal husbandry industries. Due to their extensive use, antibiotics have a very high level of residues in animals, feces, and water and soil, posing potential hazards to human health. my country's relevant standards stipulate that the residues of tetracycline antibiotics in animal-derived foods shall not exceed 100 μg / kg. Tetracycline is one of the tetracycline antibiotics, and it has residues in many media such as milk and fish. At present, the commonly used detection methods mainly include microbial method, enzyme-linked immunosorbent assay, high performance liquid chromatography and liquid chromatography-tandem mass spectrometry etc. Some of these method...

Claims

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Application Information

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IPC IPC(8): G01N27/333
Inventor 赵慧敏王红涛全燮陈硕
Owner DALIAN UNIV OF TECH
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