Method for detecting enrofloxacin in water body

Abstract

The invention discloses a method for detecting enrofloxacin in a water body. The method comprises the steps of reacting terephthalaldehyde with 1,3,5tri(4-aminophenyl) benzene to generate TAPB-PDA-COFs; carrying out a reaction on TAPB-PDA-COFs, chloroauric acid and sodium citrate to obtain a TAPB-PDA-COFs / AuNPs composite material; modifying the surface of a glassy carbon electrode with the TAPB-PDA-COFs / AuNPs composite material to prepare a modified electrode; assembling the modified electrode into a three-electrode system of an electrochemical workstation, detecting the oxidation current in the water body by using square wave stripping voltammetry, and calculating the content of enrofloxacin in the water body by comparing with a standard curve. According to the detection method disclosedby the invention, a detection result can be qualitatively obtained by directly observing whether the oxidation current is generated or not in a short time, so that the detection time of enrofloxacin is shortened, and the method is a convenient, rapid and sensitive method for detecting enrofloxacin.

Description

technical field

[0001] The invention belongs to the field of analytical chemistry, and in particular relates to a highly sensitive method for trace detection of enrofloxacin in water. Background technique

[0002] The third-generation quinolone enrofloxacin is only partially metabolized in the body, and part of the substrate and its metabolites are excreted through urine and feces. These residues may cause various toxic effects and pollute the environment. The toxicity of enrofloxacin includes allergy, immunopathology, mutagenicity, carcinogenicity, liver toxicity, kidney disease, abnormal reproductive function, bone marrow toxicity, and even human anaphylactic shock.

[0003] At present, the analysis and detection methods for antibiotics in the environment mainly include high-performance liquid chromatography, gas chromatography-mass spectrometry, liquid chromatography-mass spectrometry, capillary electrophoresis, and high-performance thin-layer chromatography. However, th...

Examples

Embodiment 1

[0047] The preparation of the modified electrode used in the detection of enrofloxacin in the water body of the present invention and the detection effect of the modified electrode on enrofloxacin under different incubation times:

[0048] (1) Preparation of TAPB-PDA-COFs: PDA (0.05 g) and TAPB (0.095 g) were added to 50 mL DMSO, ultrasonicated for 5 min to obtain a uniformly dispersed solution; under ultrasonic conditions, 1.8 mL acetic acid, sonicated for 10 min; then the reaction solution was sealed and incubated at room temperature for 30 min; finally centrifuged (10000 rpm for 10 min), washed (washed three times with tetrahydrofuran and methanol respectively), dried (dried at 55 °C under vacuum for 6 h) Grinding into powder, and the obtained TAPB-PDA-COFs powder is stored under dry conditions at room temperature until use.

[0049] (2) Preparation of TAPB-PDA-COFs / AuNPs composite material: Take 20 mg of TAPB-PDA-COFs powder prepared in step (1) into 20 mL of ultrapure wat...

Embodiment 2

[0054] The preparation of the modified electrode used in the detection of enrofloxacin in the water body of the present invention and the detection effect of the modified amount of the working electrode material on enrofloxacin:

[0055] (1) Preparation of TAPB-PDA-COFs: PDA (0.05 g) and TAPB (0.095 g) were added to 50 mL DMSO, ultrasonicated for 5 min to obtain a uniformly dispersed solution; then 1.8 mL of acetic acid was slowly added under ultrasonic conditions, and ultrasonically 10 min; then the reaction solution was sealed and incubated at room temperature for 30 min; finally centrifuged (10000 rpm for 10 min), washed (washed three times with tetrahydrofuran and methanol), dried (dried at 55 °C for 6 h under vacuum), Grinding into powder, the obtained TAPB-PDA-COFs powder is stored at room temperature and under dry conditions until use.

[0056] (2) Preparation of TAPB-PDA-COFs / AuNPs composite material: 20 mg of TAPB-PDA-COFs powder prepared in step (1) was added into 20...

Embodiment 3

[0061] A method for detecting enrofloxacin in water bodies of the present invention specifically comprises the following steps:

[0062] (1) Preparation of TAPB-PDA-COFs: PDA (0.05 g) and TAPB (0.095 g) were added to 50 mL DMSO, ultrasonicated for 5 min to obtain a uniformly dispersed solution; under ultrasonic conditions, 1.8 mL acetic acid, sonicated for 10 min; then the reaction solution was sealed and incubated at room temperature for 30 min; finally centrifuged (10000 rpm for 10 min), washed (washed three times with tetrahydrofuran and methanol respectively), dried (dried at 55 °C under vacuum for 6 h) Grinding into powder, and the obtained TAPB-PDA-COFs powder is stored under dry conditions at room temperature until use.

[0063] (2) Preparation of TAPB-PDA-COFs / AuNPs composite material: 20 mg of TAPB-PDA-COFs powder prepared in step (1) was added into 20 mL of ultrapure water, ultrasonically dispersed for 10 min; then 2.4 mL of 40 mM sodium citrate aqueous solution, he...

technical field

[0001] The invention belongs to the field of analytical chemistry, and in particular relates to a highly sensitive method for trace detection of enrofloxacin in water. Background technique

[0002] The third-generation quinolone enrofloxacin is only partially metabolized in the body, and part of the substrate and its metabolites are excreted through urine and feces. These residues may cause various toxic effects and pollute the environment. The toxicity of enrofloxacin includes allergy, immunopathology, mutagenicity, carcinogenicity, liver toxicity, kidney disease, abnormal reproductive function, bone marrow toxicity, and even human anaphylactic shock.

[0003] At present, the analysis and detection methods for antibiotics in the environment mainly include high-performance liquid chromatography, gas chromatography-mass spectrometry, liquid chromatography-mass spectrometry, capillary electrophoresis, and high-performance thin-layer chromatography. However, th...

Examples

Embodiment 1

[0047] The preparation of the modified electrode used in the detection of enrofloxacin in the water body of the present invention and the detection effect of the modified electrode on enrofloxacin under different incubation times:

[0048] (1) Preparation of TAPB-PDA-COFs: PDA (0.05 g) and TAPB (0.095 g) were added to 50 mL DMSO, ultrasonicated for 5 min to obtain a uniformly dispersed solution; under ultrasonic conditions, 1.8 mL acetic acid, sonicated for 10 min; then the reaction solution was sealed and incubated at room temperature for 30 min; finally centrifuged (10000 rpm for 10 min), washed (washed three times with tetrahydrofuran and methanol respectively), dried (dried at 55 °C under vacuum for 6 h) Grinding into powder, and the obtained TAPB-PDA-COFs powder is stored under dry conditions at room temperature until use.

[0049] (2) Preparation of TAPB-PDA-COFs / AuNPs composite material: Take 20 mg of TAPB-PDA-COFs powder prepared in step (1) into 20 mL of ultrapure wat...

Embodiment 2

[0054] The preparation of the modified electrode used in the detection of enrofloxacin in the water body of the present invention and the detection effect of the modified amount of the working electrode material on enrofloxacin:

[0055] (1) Preparation of TAPB-PDA-COFs: PDA (0.05 g) and TAPB (0.095 g) were added to 50 mL DMSO, ultrasonicated for 5 min to obtain a uniformly dispersed solution; then 1.8 mL of acetic acid was slowly added under ultrasonic conditions, and ultrasonically 10 min; then the reaction solution was sealed and incubated at room temperature for 30 min; finally centrifuged (10000 rpm for 10 min), washed (washed three times with tetrahydrofuran and methanol), dried (dried at 55 °C for 6 h under vacuum), Grinding into powder, the obtained TAPB-PDA-COFs powder is stored at room temperature and under dry conditions until use.

[0056] (2) Preparation of TAPB-PDA-COFs / AuNPs composite material: 20 mg of TAPB-PDA-COFs powder prepared in step (1) was added into 20...

Embodiment 3

[0061] A method for detecting enrofloxacin in water bodies of the present invention specifically comprises the following steps:

[0062] (1) Preparation of TAPB-PDA-COFs: PDA (0.05 g) and TAPB (0.095 g) were added to 50 mL DMSO, ultrasonicated for 5 min to obtain a uniformly dispersed solution; under ultrasonic conditions, 1.8 mL acetic acid, sonicated for 10 min; then the reaction solution was sealed and incubated at room temperature for 30 min; finally centrifuged (10000 rpm for 10 min), washed (washed three times with tetrahydrofuran and methanol respectively), dried (dried at 55 °C under vacuum for 6 h) Grinding into powder, and the obtained TAPB-PDA-COFs powder is stored under dry conditions at room temperature until use.

[0063] (2) Preparation of TAPB-PDA-COFs / AuNPs composite material: 20 mg of TAPB-PDA-COFs powder prepared in step (1) was added into 20 mL of ultrapure water, ultrasonically dispersed for 10 min; then 2.4 mL of 40 mM sodium citrate aqueous solution, he...

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