research article: a confirmatory method of tetracycline antibiotics in chinese mitten crab (eriocheir sinensis) with ultra-performance liquid chromatography tandem high-resolution mass spectrometry

A confirmatory method for the determination of tetracycline antibiotics (tcs) in chinese mitten crab has been developed for the first time. the method comprises two stages: pretreatment of the samples and instrumental analysis. the samples are treated with na2edta–mcilvaine buffer followed by extraction. the extract is then analyzed with ultra-performance liquid chromatography tandem high-resolution mass spectrometry (uplc-hrms). four mostly used tcs, including tetracycline, oxytetracycline, chlortetracycline, and doxycycline, were detected in 10 min. the specificity was confirmed via the retention time and their high-resolution mass spectra. in the range of 50-500 μg/kg, the linear regression coefficients (r2) for all analytes were greater than 0.9985. recoveries at three concentration levels were between 90.3% and 106.2%. the within-laboratory reproducibility was precise. the decision limit (ccα) and detection capability (ccβ) of the method were determined using the permitted limit (100 μg/kg) of tcs. the detection results of tcs in 12 batches of chinese mitten crab showed that no target residues were detected. this comprehensive method is compliant with the 2002/657/ec decision. it could be applied for the determination of tcs in chinese mitten crab samples and potentially in other aquatic products.