Determination of 80 Veterinary Drug Residues and Their Metabolites in Beef by HPLC-MS/MS(HPLC-MS/MS法同时测定牛肉中80种兽药及其代谢物)
摘要
In order to comprehensively investigate the risk of veterinary drug residue in beef in Ningxia, in this study, 12 types of drugs were screened and identified from three aspects:banned and stopped drugs prescribed by the Ministry of Agriculture and Rural Affairs, the drugs with the maximum residue limits specified in the GB 31650—2019“National Food Safety Standards Maximum Residue Limits of Veterinary Drugs in Food”, and drugs used in large quantities in Ningxia's breeding process. Using simple and fast pre-processing methods and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) multi-reaction monitoring and analysis technology, a rapid detection method was established which could simultaneously analyze and detect 12 types of 80 veterinary drugs and their metabolites with one injection. The sample was purified by Oasis PRiME HLB solid phase extraction column, separated by Waters HSS T3 chromatographic column, monitored by multi-reaction monitoring mode, and quantified by matrix matching external standard method. The results showed that 80 veterinary drugs and their metabolites showed a good linear relationship in the concentration range of matrix matching standard solution 1.0-50.0μg/L, with the correlation coefficients greater than 0.990. The quantitative limits of the method was 2.0-5.0μg/kg, and the average recoveries in the range of 2.0-100.0μg/kg were 60%-103%, and the relative standard deviation was less than 20% (n=5). This method was used to detect 40 pieces of commercially available beef, of which 4 pieces of beef were detected with veterinary drug residues, including oxytetracycline (54.5μg/kg), sulfamethoxine (23.3μg/kg and 35.4μg/kg), and enrofloxacin (118μg/kg). The positive samples were re-examined using GB/T 21317—2007, GB/T 20759—2006, and GB/T 21312—2007 methods, and the results were consistent. The verification showed that the qualitative and quantitative results of the detection method were accurate, reliable, sensitive,