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.