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Synchronous detection method of tetracyclines, fluoroquinolones and sulfonamide antibiotics remained in water body

A technology of fluoroquinolones and tetracyclines, which is applied in the simultaneous detection of fluoroquinolones and sulfonamide antibiotics, and the field of residual tetracyclines in water, achieving the effects of small standard deviation, high accuracy and sensitivity, and low environmental toxicity

Inactive Publication Date: 2015-06-24
CHINA UNIV OF GEOSCIENCES (WUHAN)
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the existing studies are aimed at the detection of a small number of antibiotics and most of them belong to the same type of antibiotics. Although the purpose of simultaneous detection has been achieved, the method still has limitations.

Method used

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  • Synchronous detection method of tetracyclines, fluoroquinolones and sulfonamide antibiotics remained in water body
  • Synchronous detection method of tetracyclines, fluoroquinolones and sulfonamide antibiotics remained in water body
  • Synchronous detection method of tetracyclines, fluoroquinolones and sulfonamide antibiotics remained in water body

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1 water sample pretreatment

[0023] All glassware used in the experiment were washed with organic washing liquid, and then washed with tap water and ultrapure water eight times after standing for 4 hours. During the experiment, the samples were protected from direct exposure to the light source, and some of the glassware used was brown. Some steps that required observation of the sample phenomenon used colorless glassware but covered the surface with aluminum foil to avoid light.

[0024] For different types of water samples, different volumes of samples can be measured and concentrated to reach a detectable concentration. After a series of experiments, groundwater is 1L, river water is 0.5L, and wastewater is 0.1L. Weigh a certain volume of water sample with a measuring cylinder, pass the water sample through a glass filter equipped with a 0.45 μm glass fiber filter membrane, collect the filtered water sample, and adjust the filtered water sample to pH 3-4 ...

Embodiment 2

[0025] Embodiment 2 solid phase extraction method

[0026] (1) Activation of solid phase extraction column

[0027] Waters Oasis HLB 60mg / 3mL solid phase extraction column was used for extraction. Add 6mL of chromatographically pure methanol solution to the solid-phase extraction column before use, and let the methanol solution slowly pass through the solid-phase substance under the action of gravity to activate. In order to avoid the influence of the residual methanol solvent in the solid phase on the enrichment of the target compound in the water sample, 6 mL of ultrapure water was added to it, and the solid phase was also passed through the solid phase under the action of gravity to complete the activation.

[0028] (2) Import pretreated samples

[0029] Pass the pretreated water sample into the activated solid-phase extraction column, and through the flow rate control comparison experiment, the present invention selects the flow rate as groundwater 5mL / min, river water 2...

Embodiment 3

[0036] Embodiment 3: HPLC-MS / MS detection method establishes

[0037] For trace antibiotics in the sample, high-performance liquid chromatography tandem mass spectrometry was used for detection, equipped with a high-performance autosampler, binary pump, constant temperature chromatographic column chamber, and variable wavelength detector. The specific detection parameters are shown in Table 1 below.

[0038] Table 1 High performance liquid chromatography tandem mass spectrometry (HPLC-MS / MS) detection parameters

[0039]

[0040]

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PUM

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Abstract

The invention belongs to the technical field of detection of enrichment of remained antibiotics in a water body environment, and particularly relates to a synchronous detection method of tetracyclines, fluoroquinolones and sulfonamide antibiotics remained in the water body. The detection method comprises the following steps: (1) performing water sample pretreatment; (2) performing small-column enrichment of target antibiotics by using solid-phase extraction; (3) detecting on a machine by using high performance liquid chromatography and tandem mass spectrum. According to the method, once the sample feeding is carried out at one time, multiple antibiotics in the water body can be detected at the same time, the time consumption of a detection process is reduced, the detection accuracy and sensitivity are increased, the detection limit is low, and the condition of the trace amount of remained antibiotics in the water body environment can be detected; meanwhile, the detection method is convenient to operate and low in environment toxicity and is low in using amount of organic reagents.

Description

technical field [0001] The invention belongs to the technical field of enrichment detection of residual antibiotics in water environment, and in particular relates to a method for synchronous detection of residual tetracyclines, fluoroquinolones and sulfonamide antibiotics in water. Background technique [0002] Antibiotics, as emerging pollutants in the environment, have attracted a lot of attention in recent years. Due to their long-term continuous input into the environment, the academic circles call them pseudo-persistent organic compounds. In China, the abuse of antibiotics has been serious in recent years, and they are widely used in animal husbandry and pharmaceutical industries. There are a wide range of sources of antibiotics in the environment, including the untreated discharge of production sewage from pharmaceutical factories and improper disposal of expired drugs, which will cause antibiotic residues in the environment. In addition, studies have shown that 30%-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 姚林林王焰新童蕾
Owner CHINA UNIV OF GEOSCIENCES (WUHAN)
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