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Method for detecting sulfonamide and beta-lactam antibiotics in livestock and poultry breeding wastewater

A technology for livestock and poultry breeding wastewater and detection methods, which is applied in the field of detection of sulfonamides and β-lactam antibiotics in livestock and poultry breeding wastewater, can solve problems such as the complexity of the breeding wastewater matrix, achieve less time-consuming detection process, and shorten the detection cycle , handle simple effects

Pending Publication Date: 2020-08-07
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the matrix of aquaculture wastewater is complex and contains many types of antibiotics. It is the goal of researchers to establish a rapid and accurate analysis method for various antibiotics.

Method used

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  • Method for detecting sulfonamide and beta-lactam antibiotics in livestock and poultry breeding wastewater
  • Method for detecting sulfonamide and beta-lactam antibiotics in livestock and poultry breeding wastewater

Examples

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Effect test

Embodiment 1

[0061] The present embodiment provides a method for detecting sulfonamides and β-lactam antibiotics in livestock and poultry wastewater, comprising the following steps:

[0062] Pre-treatment: Centrifuge and filter the water sample to be tested in turn, then add deionized water to the obtained filtrate to dilute, add Na 2 EDTA, and adjust the pH to 3 to obtain the pre-treated water sample;

[0063] Enrichment and purification: the pre-treated water sample is subjected to solid phase extraction, and then the solid phase extraction column subjected to the solid phase extraction is subjected to negative pressure rinsing and normal pressure elution, and the eluate is collected, and the The eluent is blown with nitrogen, and then constant volume is obtained to obtain the antibiotic solution to be tested;

[0064] Antibiotic detection: adopt high-performance liquid chromatography tandem mass spectrometry (HPLC-MS / MS) method to carry out the content detection of antibiotic to descri...

Embodiment 2

[0072] The present embodiment provides a method for detecting sulfonamides and β-lactam antibiotics in livestock and poultry wastewater, comprising the following steps:

[0073] 1) Pretreatment: Centrifuge the water sample to be tested at 3000r / min for 5min, and filter it through a glass fiber filter membrane with a pore size of 0.47mm to obtain the filtrate, then add deionized water to dilute, add Na 2 EDTA, and adjust the pH to 3 to obtain the pre-treated water sample;

[0074] 2) Enrichment and purification: performing solid-phase extraction on the pre-treated water sample, then performing negative-pressure rinsing and normal-pressure elution on the solid-phase extraction column of the solid-phase extraction, and collecting the eluate , blowing the eluent with nitrogen, and then constant volume to obtain the antibiotic solution to be tested;

[0075] In this embodiment, the solid-phase extraction treatment is: enrich the above-mentioned water sample with a solid-phase extr...

Embodiment 3

[0094] In this example, the detection method of the present invention is subjected to a standard addition recovery experiment: in this example, the internal standard method is used to determine antibiotics, and the method of adding target antibiotics to actual livestock and poultry wastewater is used to consider the standard addition recovery rate of the method.

[0095] The concrete steps of this embodiment are as follows:

[0096] (1) Pretreatment: take the biogas slurry and centrifuge at 3000r / min for 5min in a glass centrifuge tube, and filter through a glass fiber membrane to obtain the filtrate; accurately take 50mL of the filtrate and dilute it to 500mL with deionized water, add 10μL of 10mg / L Sulfa internal standard and 10μL 10mg / L β-lactam internal standard; add 0.2g Na 2 EDTA was stirred until dissolved; and washed with 2.5M H 2 SO 4 Adjust the pH of the solution to 3.

[0097] (2) Solid-phase extraction (SPE) (ANPEL, Polysery HLB) enrichment and purification proc...

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Abstract

The invention discloses a method for detecting sulfonamide and beta-lactam antibiotics in livestock and poultry breeding wastewater. The method comprises the following steps: sequentially centrifugingand filtering a to-be-detected water sample; adding deionized water into the obtained filtrate for dilution; adding Na2EDTA, adjusting the pH, carrying out solid-phase extraction treatment on the obtained pre-treated water sample, carrying out negative-pressure leaching treatment and normal-pressure elution treatment on a solid-phase extraction column subjected to the solid-phase extraction treatment, collecting eluent, and then carrying out nitrogen blowing and constant volume treatment to obtain an antibiotic solution to be detected; and carrying out antibiotic content detection on the antibiotic solution to be detected by adopting a high performance liquid chromatography-tandem mass spectrometry method. According to the detection method disclosed by the invention, a solid phase extraction-liquid chromatography tandem mass spectrometry method is adopted, and various process conditions and parameters are selected and determined, so that the detection method can be used for rapidly and accurately detecting antibiotics in water and detecting sulfonamide and beta-lactam antibiotics in the livestock and poultry breeding wastewater at the same time.

Description

technical field [0001] The invention relates to the technical field of analysis and detection of trace organic matter in water environment, in particular to a detection method of sulfonamide and β-lactam antibiotics in livestock and poultry breeding wastewater. Background technique [0002] Veterinary antibiotics have been widely used in disease prevention, treatment and growth promotion in the livestock and poultry industry. The average consumption of veterinary antibiotics in my country reaches about 6,000 tons per year. It is estimated that about 75% of antibiotics are not utilized by animals, and are excreted into the environment in the form of original drugs or metabolites through urine or feces, leading to an increase in the level of drug resistance in the environment and becoming important new environmental pollutants. Seriously endanger the ecological environment and human health. The concentration of organic matter in livestock and poultry wastewater is high, and t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/08G01N30/14G01N30/34G01N30/72
CPCG01N30/02G01N30/06G01N30/08G01N30/14G01N30/34G01N30/72G01N2030/045G01N2030/062
Inventor 张卫刘淋万江卞浩李倩男沈根祥胡双庆钱晓雍张洪昌
Owner EAST CHINA UNIV OF SCI & TECH
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