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Magnetic nano-microsphere and method for extracting and analyzing five trace quinolone antibiotics in water body by virtue of magnetic nano-microsphere

A technology of fluoroquinolones and magnetic nanometers, which is applied to the analysis of materials, chemical instruments and methods, and material separation. It can solve the problems of large consumption of organic solvents, environmental pollution, and low specificity, and achieve optimal extraction time and shorten the extraction time. The best results in analysis time and extraction performance

Inactive Publication Date: 2018-11-27
JILIN INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Traditional sample pretreatment techniques such as liquid-liquid extraction have long operating time, low recovery rate, poor repeatability, and use a large amount of organic solvents to cause serious pollution to the environment, which is not in line with contemporary green chemistry.
Solid phase extraction (SPE) is currently the most widely used sample pretreatment technology. This method has the problems of large consumption of organic solvents, low specificity, high price, and SPE cartridges can only be used once. A new type of extraction material with strong clenbuterol enrichment ability, simple preparation method and low price

Method used

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  • Magnetic nano-microsphere and method for extracting and analyzing five trace quinolone antibiotics in water body by virtue of magnetic nano-microsphere
  • Magnetic nano-microsphere and method for extracting and analyzing five trace quinolone antibiotics in water body by virtue of magnetic nano-microsphere
  • Magnetic nano-microsphere and method for extracting and analyzing five trace quinolone antibiotics in water body by virtue of magnetic nano-microsphere

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Effect test

Embodiment 1

[0039] The present embodiment provides a kind of preparation method of magnetic nano microsphere, comprises the following steps:

[0040] Weigh 0.3g Cys and dissolve in 35mL water; then add 0.3g Fe 3 o 4 Ultrasound for 15 minutes to fully dissolve; magnetic separation, pour off the supernatant, add deionized water and place in an ultrasonic cleaner to sonicate and wash. Add 1.7016g of tetrabutyl titanate; add 0.90575g of 2-aminoterephthalic acid, add 54mL of dimethylformamide and 6mL of methanol; ultrasonically dissolve without particles, add to a 100mL hydrothermal synthesis kettle, put Heat in a constant temperature oven at 120°C for 24 hours. After the reaction is complete, pour all the materials in the kettle into a beaker, add N,N-dimethylformamide, and place it in an ultrasonic cleaner for repeated cleaning. After the supernatant was clarified, absolute ethanol was added for washing. After cleaning, it is placed in a vacuum drying oven and fully dried to obtain taup...

Embodiment 2

[0048] This embodiment provides a method for extracting traces of fluoroquinolone antibiotics in water using the magnetic nanospheres described in Example 1, comprising the following steps:

[0049] 25mg of the magnetic nanospheres Fe 3 o 4 @Cys @MIL125-NH 2 Disperse in 50mL of the water sample to be tested, adjust the pH to 7.0, vortex for 20min, so that the fluoroquinolone antibiotics are completely adsorbed on the magnetic nanospheres, then discard the supernatant, add 2mL of eluent (ammonia water: methanol = 3:7), elute the magnetic nanospheres, vortex again for 20 minutes for magnetic separation, take the supernatant, blow dry with nitrogen, and use liquid chromatography mobile phase to make the volume to 1mL, that is to complete the trace fluorine in the water Extraction and elution of quinolone antibiotics. Take 500μL of this solution directly in the sample bottle for UPLC determination.

Embodiment 3

[0051] The effect of different dosages of magnetic nanospheres on the extraction efficiency of trace fluoroquinolone antibiotics in water was investigated.

[0052] According to the method described in Example 2 to extract the fluoroquinolone antibiotics in the water body, the difference is that the magnetic nanosphere Fe 3 o 4 @Cys @MIL125-NH 2 The masses are 5 mg, 10 mg, 15 mg and 25 mg, respectively. Depend on Figure 4 As shown, with the increase of the mass of the magnetic nanospheres, the extraction efficiency of the added fleroxacin, ofloxacin, ciprofloxacin, enrofloxacin, and safloxacin increased significantly until the mass of the adsorbent When reaching 25mg, the extraction efficiency is greater than 95%. Therefore, the quality of the magnetic nano-microspheres selected by the present invention is 25mg.

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Abstract

The invention provides a magnetic nano-microsphere and a method for extracting and analyzing five trace quinolone antibiotics in a water body by virtue of the magnetic nano-microsphere. The magnetic nano-microsphere is Fe3O4@Cys@MIL125-NH2. By taking a magnetic solid phase extraction technique as the basis and the magnetic nano-microsphere as an adsorbent, the quinolone antibiotics in a to-be-tested water body are pretreated and enriched, so that the sensitivity of the method for detecting the trace quinolone antibiotics in the water body is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of water quality detection, and particularly relates to a magnetic nano-microsphere and a method for extracting and analyzing five trace fluoroquinolone antibiotics in water bodies. Background technique [0002] Fluoroquinolones are a class of synthetic antibiotics (FQs). Common FQs drugs include safloxacin, ofloxacin, ciprofloxacin, enrofloxacin, fleroxacin, dafloxacin mesylate, sarafloxacin hydrochloride and difloxacin hydrochloride, among which the latter 4 kinds are special drugs for veterinary animals. This class of antibiotics is a new type of pollutant that has become a non-negligible part of environmental governance. [0003] Fluoroquinolone antibiotics for human medical use are discharged into the sewage system by feces and urine excreta produced by the human body. Such antibiotics are difficult to degrade, so they are deposited in the sludge of the sewage system, and the sludge of the sewage plan...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/08B01J20/281B01J20/28B01J20/30
CPCB01J20/28004B01J20/28009B01J20/28021B01J20/281G01N30/02G01N30/06G01N30/08G01N2030/062
Inventor 连丽丽张鑫洋吕进义娄大伟王希越张浩高文秀马先红
Owner JILIN INST OF CHEM TECH
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