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.
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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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