Rapid detection of antibiotics and their metabolite in marine biological samples by QuEChERS with liquid chromatography-tandem mass spectrometry

In this study, 19 kinds of antibiotics in five categories (tetracyclines, β-lactams, macrolides, sulfonamides and quinolones) and 5 antibiotic metabolites were included as target analytes. A pretreatment extraction method for antibiotics and their metabolites residues in typical marine organisms (croaker, shrimp, clam) was established. The extraction recoveries of the targets under different extraction methods (QuEChERS method, Ultrasonic extraction-column purification method) were compared, and the salting-out and adsorbents in the pretreatment process were optimized. The results showed that the recovery efficiency of the QuEChERS method was better than that of the Ultrasonic extraction-column purification method. In addition, the QuEChERS method using sodium chloride and sodium sulfate as salting agents as well as C18 as adsorbents showed a better extraction efficiency than the QuEChERS method using magnesium sulphate and trisodium citrate as salting agents. The detection limits of the optimized method for 24 antibiotics and metabolites were 0.04～3.31 µg/kg, and the recoveries by the method were 60.23%～119.88% with the relative standard deviations (RSD) of 0.10%～29.79%. The study provides technical support for the study of the residual characteristics and environmental behavior of antibiotics and their metabolites in marine organisms.