Abstract:In order to comprehensively investigate the risk of veterinary drug residues in black bone chicken, a rapid detection method for simultaneous analysis of 39 veterinary drugs and their metabolites in three categories was established by using low-temperature ultrasonic extraction, solid-phase extraction pretreatment technology and ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The samples were extracted by mcllvaine-Na2EDTA and phosphate buffer at low temperature, cleaned by oasis HLB solid phase extraction column, separated by T3 column, and quantified by matrix matching external standard method. 39 veterinary drugs and their metabolites showed a good linear relationship in the concentration range of matrix matching external standard solution 2.0～100 μg/L, the correlation coefficient was greater than 0.990, the detection limit was 2 μg/kg, and the limit of quantification was 10 μg/kg. The average recovery of the method in the range of 10～100 μg/kg was 70%～103%, and the relative deviation (n = 5) was less than 15%. The method has high sensitivity, reliable qualitative and quantitative results, and can meet the requirements for the detection and analysis of veterinary drug residues in black bone chicken. Using this method, 60 samples of black bone chicken sold in the market were tested. The results showed that fluoroquinolones, tetracyclines and sulfonamides were detected in commercial black bone chickens, and enrofloxacin (sum of ciprofloxacin), trimethoprim and dimethyloprim exceeded the maximum residue limit, which were 2 enrofloxacin (153.187, 174.979 μg/kg) and 2 parts of trimethoprim (55.007, 111.391 μg/kg) and 2 parts of trimethoprim (153.779、189.801 μg/kg). This shows that there is a certain risk of the residue of sulfonamides antibiotics in black bone chicken on the market, and it is necessary to strengthen the restraint of the safe use of antibiotics in black bone chicken breeding.
