Establishment and dietary risk assessment of UPLC-MS/MS detection method for 16 quinolone antibiotics in freshwater fish
Objective:This study aimed to establish a method for the simultaneous determination of 16 quinolones in freshwater fish by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)and then analyze the effect of three different cooking methods(by boiling,steaming and frying)on the residues of quinolone antibiotics.Methods:Samples were ultrasonic extracted with acetonitrile(with 4％formic acid)and purified with C18 solid phase extraction column.The chromatographic separation was performed on a Waters ACQUITY UPLC BEH C18(1.7 μm,2.1 mm × 100 mm)column,with 0.1％formic acid water-acetonitrile as mobile phase for gradient elution.Mass spectrometry(ESI+)was monitored by multiple reaction ions and quantified by internal standard method.Results:16 quinolones showed a clear linear relationship between 2.0 ng/mL and 50 ng/mL,and the correlation coefficient was greater than 0.998 49.The limits of detection quantification were 0.3～4.1 μg/kg and 0.9～11.0 μg/kg,respectively.Average recoveries in matrices at low,medium,and high spiked levels ranged from 79.0％to 104.7％,with a standard deviation of 1.0％to 8.1％.There was no significant difference in the residues of 16 quinolones between the fish meat-positive samples of three different cooking methods and the control.Conclusion:The method was simple,rapid,and sensitive,and met the high-throughput screening and dietary risk assessment of quinolone antibiotics in freshwater fish.
国家科技期刊平台
NSTL
万方数据
维普
