Method for simultaneously detecting 15 antibiotics in aquaculture water body by solid-phase extraction pretreatment combined with liquid chromatography-mass spectrometry technology

A LC/MS and aquaculture technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of limited quantity and types of detection antibiotics, unstable detection methods, limited recovery rate, etc., to improve selectivity and enrichment. Set multiples, the results are true and reliable, and the recovery rate is high.

Inactive Publication Date: 2019-02-15
SHANGHAI ACADEMY OF ENVIRONMENTAL SCIENCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, there is no complete and reliable detection method for the separation, enrichment and co-detection of various antibiotics in aquaculture water. Therefore, there is an urgent need for a complete and reliable detection method that has stable detection results, low interference, fast, efficient, sensitive, and accurate detection of as many antibiotic residues as possible in aquaculture water, including separation, enrichment, and co-detection. detection method

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  • Method for simultaneously detecting 15 antibiotics in aquaculture water body by solid-phase extraction pretreatment combined with liquid chromatography-mass spectrometry technology
  • Method for simultaneously detecting 15 antibiotics in aquaculture water body by solid-phase extraction pretreatment combined with liquid chromatography-mass spectrometry technology
  • Method for simultaneously detecting 15 antibiotics in aquaculture water body by solid-phase extraction pretreatment combined with liquid chromatography-mass spectrometry technology

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Experimental program
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Effect test

Embodiment 1

[0042] Embodiment 1: solid phase extraction elution solvent selection

[0043] Using the internal standard method, determine the elution solvent in the detection method of the solid phase extraction pretreatment of the present invention combined with the liquid chromatography-mass spectrometry technology, and measure the standard addition recovery rate of 15 kinds of antibiotics in the aquaculture water body by three different elution solvents . In the standard addition recovery experiment, tap water was used as a sample: 10 μL of antibiotic mixed standard solution (the antibiotic mixed standard solution was a mixed standard solution of 15 kinds of antibiotics, wherein the concentrations of the 15 kinds of antibiotics were respectively 10 mg / L) was added to the sample.

[0044] The method for the simultaneous detection of 15 kinds of antibiotics in aquaculture water by the solid-phase extraction pretreatment of the present invention in combination with liquid chromatography-ma...

Embodiment 2

[0058] Embodiment 2: standard addition recovery experiment

[0059] The internal standard method was used to test the recovery rates of 15 kinds of antibiotics in the aquaculture water body measured by the detection method of the solid phase extraction pretreatment combined with the liquid chromatography-mass spectrometry technique of the present invention. The standard addition recovery experiment takes tap water as a sample: add 10 μL and 20 μL antibiotic mixed standard solutions to the sample respectively (this antibiotic mixed standard solution is a mixed standard solution of 15 kinds of antibiotics, wherein the concentration of 15 kinds of antibiotics is 10 mg / L respectively ).

[0060]The method for the simultaneous detection of 15 kinds of antibiotics in aquaculture water by the solid-phase extraction pretreatment of the present invention in combination with liquid chromatography-mass spectrometry is specifically implemented according to the following steps:

[0061] S...

Embodiment 3

[0089] Embodiment 3: actual aquaculture water sample antibiotic content determination

[0090] Determination of the concentration of 15 antibiotics in two aquaculture farms

[0091] Collect water samples from a crab farm and shrimp farm in Shanghai, first use the method of step 1 of the present invention to carry out sample pretreatment, and then use the solid phase extraction method of step 2 of the present invention to carry out enrichment and purification pretreatment, and then use the method of the present invention The high-performance liquid chromatography tandem mass spectrometer in step three detects and analyzes the actual concentration of the sample, so as to investigate the applicability of the method of the present invention to different aquaculture farms.

[0092] The specific detection process is as follows:

[0093] (1) Water sample pretreatment

[0094] Set up three parallels for each sample, accurately measure 1000mL water samples into clean beakers, filter ...

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Abstract

The invention provides a method for simultaneously detecting 15 antibiotics in an aquaculture water body by solid-phase extraction pretreatment combined with a liquid chromatography-mass spectrometrytechnology. The method comprises the following steps: (1) water sample pretreatment: adding seven internal standard substances for indicating the recovery rate, namely sulfamethoxazole-13C6, norfloxacin-D5, penicillin G potassium salt-D5, achromycin-D6, olaquindox-D4, amoxicillin-13C6 and trimethoprim-D3; (2) enriching and purifying target antibiotics by using a solid-phase extraction column; (3)detecting the contents of the 15 antibiotics in seven categories in the aquaculture water body with a liquid chromatograph/mass spectrometer by adopting an internal standard method. The method provided by the invention has the benefits that with the adoption of a single-factor experiment, the residue situations of the 15 antibiotics containing 8 new antibiotics in the aquaculture water body can besimultaneously detected at a time by preferably selecting the internal standard substances and optimizing detection conditions; the method has the advantages of high precision, high sensitivity, highstability, high selectivity, low detection limit, more true and reliable detection results and the like.

Description

technical field [0001] The invention belongs to the technical field of detection of water environmental pollutants, and relates to a detection method for simultaneously detecting trace amounts of 15 commonly used antibiotics in aquaculture water, in particular to a method for simultaneous detection of aquaculture by solid-phase extraction pretreatment combined with liquid chromatography-mass spectrometry Methods of 15 antibiotics in water bodies. Background technique [0002] The use of antibiotics in aquaculture for the treatment and prevention of bacterial diseases began in the 1950s. With the rapid development of the aquaculture industry, the frequency of diseases in the breeding process is getting higher and higher, and the scope and amount of antibiotics used as veterinary drugs are increasing day by day. With the pursuit of economic benefits of aquaculture by farmers and the increase of antibiotic resistance of aquatic organisms, the dosage of antibiotics is constantl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/08G01N30/88
CPCG01N30/08G01N30/88
Inventor 张洪昌沈根祥胡双庆郭春霞钱晓雍王真汪仙仙李贞金
Owner SHANGHAI ACADEMY OF ENVIRONMENTAL SCIENCES
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