Preparation method for electrode modified material of silver indium disulphide/reduced graphene oxide and application thereof for detecting ciprofloxacin

Abstract

The invention discloses a preparation method for an electrode modified material of a silver indium disulphide / a reduced graphene oxide and an application thereof for detecting the ciprofloxacin. The preparation method comprises the following steps of: mixing the GO (graphene oxide) dispersion and the AgInS2 solution thoroughly and uniformly; transferring the GO dispersion liquid into a reaction kettle for the hydrothermal reaction to compound; obtaining the product AgInS2 / rGO by filtering, washing, and freeze-drying after the reaction is completed; using a glassy carbon electrode modified by aprepared AgInS2 / rGO nanocomposite as a working electrode, using an Ag / AgCl electrode as a reference electrode, using a platinum electrode as a counter electrode; using a 1M H2SO solution as a supporting electrolyte solution; and utilizing a differential pulse voltammetry (DPV), so that the invention can detect solutions containing different concentrations of ciprofloxacin. According to the preparation method for the electrode modified material of the silver indium disulphide / the reduced graphene oxide, the method responds quickly to the current of ciprofloxacin, and the method has a high sensitivity, a low detection limit, a strong anti-interference performance, and a high practicability.

Description

technical field

[0001] The invention relates to a detection method with low detection limit and excellent selectivity for ciprofloxacin, which belongs to the technical field of environmental pollutant detection, and specifically relates to a method for preparing an electrode modification material silver disulfide indium oxide / reduced graphene oxide and its application in detecting ciprofloxacin. Background technique

[0002] As the third-generation quinolone antibacterial drug, ciprofloxacin has broad-spectrum antibacterial activity, good bactericidal effect, and low cost. It is currently widely used in humans and animals. However, like most other antibiotic drugs, most of ciprofloxacin is excreted into the environment in the form of metabolites or even the original drug after being metabolized by patients or animals, thereby destroying the ecological balance of the environment and producing drug-resistant superbugs and other issues that seriously affect environmental safet...

Examples

Embodiment 1

[0024] Graphene oxide (GO) was prepared by modified Hummer's method.

[0025] Preparation of AgInS by precipitation method 2 , specifically: take 0.0012mol AgNO 3 Dissolve in 50mL ethylene glycol, add 0.0054mol InCl dropwise under stirring 3 4H2O, stirred for another 10 min, then added 0.75 g of thioacetamide under stirring. After continuous stirring for about 1 h, the above solution was transferred to a 100 mL three-neck flask and refluxed for 3 h. After the reaction was completed, the cloudy solution was naturally cooled to room temperature and aged for 12 h. The resulting solid was collected by filtration and washed alternately with absolute ethanol and deionized water. Finally, the product was dried in a vacuum oven for 12 hours and ground to obtain AgInS 2 Material.

[0026] By ultrasonic dispersion method, GO was prepared into a 4.3 mg / ml dispersion liquid with deionization, and 30 mL of ethylene glycol was taken, and 9.3 mL of the above-mentioned GO dispersion liq...

Embodiment 2

[0029] Graphene oxide (GO) was prepared by modified Hummer's method.

[0030] Preparation of AgInS by precipitation method 2 , specifically: take 0.0012mol AgNO 3 Dissolve in 50mL ethylene glycol, add 0.0054mol InCl dropwise under stirring 3 4H 2 0, then stirred for 10min, then added 0.75g thioacetamide under stirring. After continuous stirring for about 1 h, the above solution was transferred to a 100 mL three-neck flask and refluxed for 3 h. After the reaction was completed, the cloudy solution was naturally cooled to room temperature and aged for 12 h. The resulting solid was collected by filtration and washed alternately with absolute ethanol and deionized water. Finally, the product was dried in a vacuum oven for 12 hours and ground to obtain AgInS 2 Material.

[0031] GO was made into a 4.3mg / ml dispersion with deionization, 30mL of ethylene glycol was taken, and 9.3mL of the above-mentioned GO dispersion was added under stirring. Weigh 20mg AgInS 2 , made a sol...

Embodiment 3

[0034] Graphene oxide (GO) was prepared by modified Hummer's method.

[0035] Preparation of AgInS by precipitation method 2 , specifically: take 0.0012mol AgNO 3 Dissolve in 50mL of ethylene glycol, add 0.0054mol InCl3·4H2O dropwise under stirring, stir for another 10min, then add 0.75g of thioacetamide under stirring. After continuous stirring for about 1 h, the above solution was transferred to a 100 mL three-neck flask and refluxed for 3 h. After the reaction was completed, the cloudy solution was naturally cooled to room temperature and aged for 12 h. The resulting solid was collected by filtration and washed alternately with absolute ethanol and deionized water. Finally, the product was dried in a vacuum oven for 12 hours and ground to obtain AgInS 2 Material.

[0036] GO was made into a 4.3mg / ml dispersion with deionization, 30mL of ethylene glycol was taken, and 9.3mL of the above-mentioned GO dispersion was added under stirring. Weigh 80mg AgInS 2 , made a solu...

technical field

[0001] The invention relates to a detection method with low detection limit and excellent selectivity for ciprofloxacin, which belongs to the technical field of environmental pollutant detection, and specifically relates to a method for preparing an electrode modification material silver disulfide indium oxide / reduced graphene oxide and its application in detecting ciprofloxacin. Background technique

[0002] As the third-generation quinolone antibacterial drug, ciprofloxacin has broad-spectrum antibacterial activity, good bactericidal effect, and low cost. It is currently widely used in humans and animals. However, like most other antibiotic drugs, most of ciprofloxacin is excreted into the environment in the form of metabolites or even the original drug after being metabolized by patients or animals, thereby destroying the ecological balance of the environment and producing drug-resistant superbugs and other issues that seriously affect environmental safet...

Examples

Embodiment 1

[0024] Graphene oxide (GO) was prepared by modified Hummer's method.

[0025] Preparation of AgInS by precipitation method 2 , specifically: take 0.0012mol AgNO 3 Dissolve in 50mL ethylene glycol, add 0.0054mol InCl dropwise under stirring 3 4H2O, stirred for another 10 min, then added 0.75 g of thioacetamide under stirring. After continuous stirring for about 1 h, the above solution was transferred to a 100 mL three-neck flask and refluxed for 3 h. After the reaction was completed, the cloudy solution was naturally cooled to room temperature and aged for 12 h. The resulting solid was collected by filtration and washed alternately with absolute ethanol and deionized water. Finally, the product was dried in a vacuum oven for 12 hours and ground to obtain AgInS 2 Material.

[0026] By ultrasonic dispersion method, GO was prepared into a 4.3 mg / ml dispersion liquid with deionization, and 30 mL of ethylene glycol was taken, and 9.3 mL of the above-mentioned GO dispersion liq...

Embodiment 2

[0029] Graphene oxide (GO) was prepared by modified Hummer's method.

[0030] Preparation of AgInS by precipitation method 2 , specifically: take 0.0012mol AgNO 3 Dissolve in 50mL ethylene glycol, add 0.0054mol InCl dropwise under stirring 3 4H 2 0, then stirred for 10min, then added 0.75g thioacetamide under stirring. After continuous stirring for about 1 h, the above solution was transferred to a 100 mL three-neck flask and refluxed for 3 h. After the reaction was completed, the cloudy solution was naturally cooled to room temperature and aged for 12 h. The resulting solid was collected by filtration and washed alternately with absolute ethanol and deionized water. Finally, the product was dried in a vacuum oven for 12 hours and ground to obtain AgInS 2 Material.

[0031] GO was made into a 4.3mg / ml dispersion with deionization, 30mL of ethylene glycol was taken, and 9.3mL of the above-mentioned GO dispersion was added under stirring. Weigh 20mg AgInS 2 , made a sol...

Embodiment 3

[0034] Graphene oxide (GO) was prepared by modified Hummer's method.

[0035] Preparation of AgInS by precipitation method 2 , specifically: take 0.0012mol AgNO 3 Dissolve in 50mL of ethylene glycol, add 0.0054mol InCl3·4H2O dropwise under stirring, stir for another 10min, then add 0.75g of thioacetamide under stirring. After continuous stirring for about 1 h, the above solution was transferred to a 100 mL three-neck flask and refluxed for 3 h. After the reaction was completed, the cloudy solution was naturally cooled to room temperature and aged for 12 h. The resulting solid was collected by filtration and washed alternately with absolute ethanol and deionized water. Finally, the product was dried in a vacuum oven for 12 hours and ground to obtain AgInS 2 Material.

[0036] GO was made into a 4.3mg / ml dispersion with deionization, 30mL of ethylene glycol was taken, and 9.3mL of the above-mentioned GO dispersion was added under stirring. Weigh 80mg AgInS 2 , made a solu...

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