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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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.: 2

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

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Example Embodiment

[0021] In Example 1, a platinum electrode was used as the electrode substrate, and a tetracycline molecularly imprinted polymer membrane electrode was prepared by a thermal polymerization method.

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

[0023] Use Al for platinum electrode 2 O 3 After the powder is polished, it is ultrasonically cleaned with ethanol and water as solutions, and dried.

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

[0025] After two thermal polymerization reactions, the elect...

Example Embodiment

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

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

[0028] The industrial pure titanium sheet (purity>99%) with a size of 20mm×30mm was polished with 350#, 800#, 1000# and 1200# emery paper in sequence, then placed in ethanol solution for ultrasonic cleaning for 3 minutes, and then deionized water Ultrasonic cleaning for 20 minutes to thoroughly clean the titanium sheet. A three-electrode system is used for electrodeposition of gold, the deposition solution is 2g / L chloroauric acid solution, the chloroauric acid solution contains 0.01mmo...

Example Embodiment

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

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

[0032] After polishing and cleaning a 20mm×30mm industrial pure titanium sheet (purity>99%) according to the process described in Example 2, a three-electrode system is used to electrodeposit platinum. 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 -0.35V (relative to the saturated calomel electrode), and the deposition time is 30...

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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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