Summary An analytical method for the determination of diclazuril residues in fish by dispersive solid phase extraction-liquid chromatography-tandem mass spectrometry was established. The sample was dehydrated by anhydrous sodium sulfate, extracted with acetonitrile by ultrasonication, concentrated under reduced pressure, degreased with n-hexane, purified by matrix-dispersed solid phase extraction, mass spectrometry by electrospray ion source negative ion scanning mode, and quantified by internal standard method. The linear relationship of diclazuril in the range of 1~100 μg/L is good, and the correlation coefficient R2>0.999. When the addition level of diclazuril was 1.00~50.0 μg/kg, the average recovery rate was between 95.4% and 108%, and the intra- and inter-assay coefficient of variation was <15%. The detection limit of diclazuril was 0.50 μg/kg. The method is sensitive, high-efficiency, simple, and reproducible, and meets the requirements for detecting the residual amount of gram-bearing residues in fish. |
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Key words: dispersive solid phase extraction, liquid chromatography-tandem mass spectrometry (LC-MS/MS), fish, diclazuril | |||||||
| Abstract: A method has been developed for the determination of diclazuril in fish by high performance liquid chromatography-mass spectrometry with dispersive solid phase extraction. Samples were dehydrated by anhydrous sodium sulfate, and extracted by acetonitrile. Then the extracts were concentrated in vacuum condition. The sample were degreased by hexane and cleaned up by dispersive solid phase extraction and then analyzed by LC-MS/MS with internal standard method. Electrospray ionization was applied and operated in the negative ion mode. The calibration curve was good linear between area and the Concentration of diclazuril from 1~100 μg/L with the correlation coefficient over 0.999. The average recoveries from spiked sample at the three concentration of 1.00, 5.00 and 50.0 μg/kg ranged from 95.4%~108% with intra and inter batch relative standard Deviation below 15%. The detection limit of diclazuril was 0.50 μg/kg. The efficient and simple method could be used to identify and Quantity the diclazuril in fish with satisfactory sensitivity and repeatability. | |||||||
| Key words: dispersive solid phase extraction high performance liquid chromatography-mass spectrometry (LC-MS/MS) fish diclazuril | |||||||
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