Method for analyzing and determining four sulfonamide antibiotics in water sample

A detection method and antibiotic technology are applied in the field of analysis and detection of four sulfonamide antibiotics in environmental water samples, which can solve the problems of improving bacterial resistance to antimicrobial agents and toxicity accumulation, and achieve good reproducibility and low detection limit. , the effect of good adsorption efficiency

Inactive Publication Date: 2020-02-28
QINGDAO TECHNOLOGICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Massive use of this antibiotic will not only increase bacterial resistance to antimicrobial agents, but also lead to toxic accumulation in organisms

Method used

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  • Method for analyzing and determining four sulfonamide antibiotics in water sample
  • Method for analyzing and determining four sulfonamide antibiotics in water sample
  • Method for analyzing and determining four sulfonamide antibiotics in water sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] The analytical detection method of four kinds of sulfonamide antibiotics in the environmental water sample that embodiment relates specifically comprises the following steps:

[0048] S1. Preparation of metal-organic framework material NH 2 -MIL-101(Fe) and NH 2 -MIL-101(Fe)- Polyvinylidene Fluoride Mixed Matrix Membrane:

[0049] (1) dissolving ferric chloride in N-N dimethylformamide (DMF), then adding aminoterephthalic acid, fully stirring and dissolving to prepare the mixture for subsequent use;

[0050] (2) react the mixture prepared in step (1) at 100-130°C in the solvothermal reactor for 24h, wash the prepared mixture in the solvothermal reactor with DMF to obtain NH 2 -MIL-101(Fe) mixed solution, and then vacuum-dried the mixed solution at 100°C to obtain the metal-organic framework material NH 2 -MIL-101(Fe) spare;

[0051] (3) Weigh NH 2 -MIL-101(Fe) powder, and dissolved in acetone to make NH 2 -MIL-101 (Fe) solution is standby, polyvinylidene fluoride ...

Embodiment 2

[0060] This embodiment investigates the main factors affecting four kinds of sulfonamide antibiotics extraction recovery rate, calculates the optimal value of each factor when the extraction recovery rate is the highest, and then measures the four kinds of sulfonamide antibiotics under the condition of the optimal value of each factor. The relevant parameters of the working curve and the detection limit and precision of the method, the specific process includes the following steps:

[0061] S1, calculate the optimal value of each factor when the extraction recovery of four kinds of sulfonamide antibiotics is the highest:

[0062] (1) The investigation of the amount of adsorbent to the extraction recovery

[0063] The present invention investigates the influence of the amount of MOF on the extraction recovery rate, and the invention weighs 40, 50, 60, 70, 80, 90, 100 mg of metal-organic framework material NH 2 -MIL-101(Fe) prepared MOF film, the concentrations of four antibiot...

Embodiment 3

[0084] Determination of the residual amount of four kinds of sulfonamide antibiotics in laboratory tap water, Laoshan Reservoir of Qingdao City, and seawater. After collecting three kinds of water samples, first filter them with rapid qualitative filter paper with a pore size of 80-120 μm, and then filter them with a 0.45 μm filter membrane; The final water sample was measured by the method described in Example 1, and the accuracy test was carried out by the method described in Example 2, and four kinds of antibiotic concentrations were prepared respectively for low, medium, and low concentrations of 1 μg / L, 10 μg / L, and 40 μg / L. The actual water samples with three concentrations higher than the standard addition recovery test were carried out, and each concentration point was measured three times, and the average value, relative standard deviation and standard addition recovery rate of the three determinations were calculated; among them, none of the three water sample blanks w...

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Abstract

The invention belongs to the field of antibiotic detection, and relates to a method for analyzing and determining four sulfonamide antibiotics in a water sample. A negative pressure suction filtrationmembrane solid phase extraction technology is utilized, and a metal organic framework material NH2-MIL-101(FE) membrane solid phase extraction-high performance liquid chromatography method is adoptedto determine four antibiotics such as sulfadiazine, sulfamethazine, sulfachloropyridazine and sulfamethoxazole in an environmental water sample. The method is simple, convenient, rapid and sensitiveto operate, and has the advantages of low detection limit, accuracy and good reproducibility; and moreover, the raw materials are cheap and easy to obtain, the material preparation process is simple,the reaction conditions are mild, the application environment is friendly, and the market prospect is wide.

Description

Technical field: [0001] The invention belongs to the field of antibiotic detection, and relates to an analysis and determination method of four kinds of sulfonamide antibiotics in a water sample, which utilizes negative pressure suction filtration membrane solid-phase extraction technology and adopts metal organic framework material NH 2 -MIL-101 (Fe) membrane solid-phase extraction-high performance liquid chromatography to determine four antibiotics, sulfadiazine, sulfamethazine, sulfachloropyridazine and sulfamethoxazole in environmental water samples. Background technique: [0002] Sulfa antibiotics (SAs) are a general term for a class of drugs with a sulfanilamide structure, and are widely used as broad-spectrum antibacterial agents in human medicine and animal husbandry. Extensive use of such antibiotics will not only increase the resistance of bacteria to antimicrobial agents, but also lead to the accumulation of toxicity in organisms. There are two main sources of su...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 马继平姜名珊李爽柴会宁
Owner QINGDAO TECHNOLOGICAL UNIVERSITY
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