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Preparation and application methods of tetracycline antibiotic multi-template molecularly imprinted magnetic composite material

A magnetic composite material and tetracycline technology are applied in the field of preparation of tetracycline antibiotic multi-template molecularly imprinted magnetic composite materials to achieve the effects of accelerated sample pretreatment process, good specific identification and fast adsorption rate

Inactive Publication Date: 2020-12-01
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to develop a novel material and corresponding technology for the simultaneous adsorption and removal of tetracycline antibiotics with good adsorption effect, high selectivity, short equilibration time and easy operation for the problems existing in the existing tetracycline adsorption materials.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026](1) Preparation of graphene oxide (GO). A modified Hummer method is used. Measure 250mL of concentrated sulfuric acid and 50mL of concentrated phosphoric acid, mix them, and place them in an ice bath. Then weigh 5.0 g flake graphite powder and 35.0 g potassium permanganate. Mix graphite powder and acid first, then slowly add potassium permanganate while maintaining the temperature below 10°C. After reacting at low temperature for 2 h, the temperature of the water bath was raised to 35°C. After reacting for 12 hours, slowly add 200 mL of ice cubes to the mixture, control the temperature of the water bath at 95°C, and react for 1 hour. After the reaction, cool to room temperature, add 1L of deionized water to dilute, and then add hydrogen peroxide to obtain a bright yellow mixed solution. Afterwards, the product was washed with concentrated hydrochloric acid and ethanol diluted 20 times, and dried under vacuum at 60 °C to obtain GO.

[0027] (2) Preparation of magneti...

Embodiment 2

[0031] Various index experiments were carried out on the composite material obtained in Example 1.

[0032] Add 20 mg of the composite material obtained in Example 1 to 20 mL of solutions containing 50 mg / L tetracycline, oxytetracycline, chlortetracycline and doxycycline at different pH values ​​to investigate the effect of pH value on the adsorption effect. The results showed that the adsorption capacity was maximum when the pH was 7.

[0033] Add 20 mg of the composite material obtained in Example 1 to 20 mL of a pH=7 solution containing 50 mg / L tetracycline, oxytetracycline, chlortetracycline and doxycycline, and investigate the effect of adsorption time on the adsorption effect. The results showed that the adsorption reached equilibrium within 60 minutes, and the adsorption process obeyed the second-order kinetics.

[0034] 20 mg of the composite material obtained in Example 1 was added to solutions containing different initial concentrations of tetracycline, oxytetracycl...

Embodiment 3

[0037] The composite material obtained in Example 1 was used for adsorption and removal of tetracycline antibiotics in environmental water samples.

[0038] Add 20 mg of the material to 20 mL of a solution containing 50 mg / L tetracycline, oxytetracycline, chlortetracycline and doxycycline, adjust the pH to 7, and shake at 200 rpm for 60 min. The adsorbent is separated from the solution under the action of an external magnetic field. The concentrations of residual tetracycline, oxytetracycline, chlortetracycline and doxycycline in the solution were determined by high performance liquid chromatography, and the removal rates of tetracycline, oxytetracycline, chlortetracycline and doxycycline were calculated. The tetracycline, oxytetracycline, chlortetracycline and doxycycline adsorbed on the material were eluted with a mixed solution of methanol:acetic acid (9:1, V:V).

[0039] The material can be reused 5 times.

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Abstract

The invention relates to preparation of a tetracycline antibiotic (tetracycline, oxytetracycline, aureomycin and doxycycline) multi-template molecularly imprinted magnetic composite material and application of the composite material in removal and detection of tetracycline antibiotics. After the surface of magnetic graphene oxide is coated with mesoporous silica, tetracycline, oxytetracycline, aureomycin and doxycycline are jointly used as template molecules, anilinomethyltriethoxysilane and N-[3-(trimethoxysilyl) propyl] ethylenediamine are jointly used as functional monomers, and a sol-gel method is adopted for surface molecular imprinting. The obtained tetracycline antibiotic multi-template molecularly imprinted magnetic composite material can be used for carrying out high-selectivity adsorption on tetracycline, oxytetracycline, aureomycin and doxycycline in a solution at the same time; the adsorption capacities are 5.9 mg / g, 5.7 mg / g, 19.5 mg / g and 11.9 mg / g respectively, adsorption equilibrium is achieved within 60 min, the adsorbent can be repeatedly used five times or more, and the material can be used for removing and detecting tetracycline antibiotics.

Description

technical field [0001] The invention belongs to the technical field of novel environmental functional materials, water treatment and analysis and detection, and specifically relates to a preparation and application method of a tetracycline antibiotic multi-template molecularly imprinted magnetic composite material. Background technique [0002] Tetracycline antibiotics are a class of broad-spectrum antibiotics produced by actinomycetes, which can be used to prevent and treat animal diseases. They are widely used pharmaceutical additives in my country at this stage. Among them, tetracycline, oxytetracycline, chlortetracycline, and doxycycline are representatives of tetracycline antibiotics, and are widely used as feed additives and veterinary drugs in animal husbandry because of their low cost and broad spectrum. After being ingested and absorbed by animals, tetracycline antibiotics have poor metabolism and cannot be digested and degraded in animals. Instead, they are excrete...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30C02F1/28C08G77/26C08J9/28G01N30/06C02F101/34C02F101/38C08L83/08
CPCB01J20/268B01J20/28009B01J20/28057C02F1/285C02F2101/34C02F2101/38C08G77/26C08J9/28C08J2383/08G01N30/06
Inventor 马晓国曾国龙
Owner GUANGDONG UNIV OF TECH
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