Establishment and Application of a UPLC-MS/MS Method for Simultaneous Determination of 39 Veterinary Drugs and Their Metabolites in Black Bone Chicken
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1.School of Animal Science and Technology, Ningxia University, Yinchuan 750021, China;2.Ningxia Veterinary Drugs and Fodder Inspection Institute, Yinchuan 750011, China;3.Husbandry Technology Extension Service Center of Yanchi Bureau of Agriculture and Rural Affairs, Wuzhong 751500, China

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    Abstract:

    [Objective] This study aims to comprehensively investigate the risk of veterinary drug residues inblack bone chicken. [Method] A method for rapid and simultaneous analysis of 39 veterinary drugs and theirmetabolites in three categories was established based on low-temperature ultrasonic extraction, solid-phaseextraction pretreatment, and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were extracted by Mcllvaine-Na2EDTA and phosphate buffer via ultrasonictreatment at low temperatures, purified by Oasis HLB solid-phase extraction column, separated by T3chromatographic column, and quantified by the matrix matching external standard method. [Result] The 39veterinary drugs and their metabolites showed good linear relationships in the matrix matching external standardsolutions with the mass concentration range of 2.0~500.0 μg/L, with the correlation coefficients greater than0.990. The limits of detection and quantification were 2.0 μg/kg and 10.0 μg/kg, respectively. The spike recoveryrates of the method ranged from 68% to 111% at fortified mass fractions of 10.0~100.0 μg/kg, and the relativestandard deviation (n=5) ranged from 0.65% to 15.12%. The method had high sensitivity and reliable qualitativeand quantitative results, meeting the requirements for the detection and analysis of veterinary drug residues inblack bone chicken. This method was then used to test 60 samples of black bone chicken sold on the market. Theresults showed that fluoroquinolones, tetracyclines, and sulfonamides were detected in commercial black bonechicken. The mass fraction of enrofloxacin, trimethoprim, and diaveridine exceeded the maximum residue limitsin two (153.187, 174.979 μg/kg), two (55.007, 111.391 μg/kg), and two (153.779, 189.801 μg/kg) samples,respectively. [Conclusion] There is a certain risk of the residues of sulfonamides in black bone chicken on themarket, and it is necessary to strengthen the supervision on use of antibiotics in black bone chicken breeding.

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DU Jiawei, LI Yongqin, JIN Shuangyuan, WANG Xueyan, WEN Hongwu, GUO Xuelian, LI Hao, XU Lihua. Establishment and Application of a UPLC-MS/MS Method for Simultaneous Determination of 39 Veterinary Drugs and Their Metabolites in Black Bone Chicken[J]. Journal of Food Science and Biotechnology,2025,44(7):161-172.

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History
  • Received:February 21,2024
  • Revised:March 19,2024
  • Adopted:
  • Online: November 03,2025
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