Department of Pharmacology and Toxicology, National Veterinary Research Institute Partyzantow 57, Pulawy, Poland.
J Sep Sci. 2018 Mar;41(5):1083-1090. doi: 10.1002/jssc.201701069. Epub 2018 Jan 10.
A method based on ultra-high performance liquid chromatography was developed and validated to detect six thyreostatic compounds: tapazole, thiouracil, methylthiouracil, dimethylthiouracil, propylthiouracil, and phenylthiouracil in faeces of bovine. Thyreostats were extracted from the matrix with a mixture of methanol and buffer (pH = 8). Next step was derivatization of analytes with 3-iodobenzylbromide. The liquid chromatographic separation of derivatives was obtained on a SB-C18 column (50 × 2.1 mm; 1.8 μm, Agilent) with gradient elution using a mobile phase consisting of acetonitrile/0.1% acetic acid within 7.5 min. The analysis was performed on a Shimadzu NEXERA X2 ultra-high performance liquid chromatograph with triple quadrupole MS 8050 instrument operating in positive electrospray ionization mode. Depending on the target compound, two or three diagnostic signals (selected reaction monitoring transitions) were monitored. The procedure was validated according to the Commission Decision 2002/657/EC. Recovery and repeatability met the performance criteria specified by this document for banned compounds. The recovery ranged from 97.5 to 110.5%, and repeatability did not exceed 14.1%. Decision limits and detection capabilities were below 10 μg/kg. The highest decision limits and detection capabilities concentrations were observed for phenylthiouracil of 3.48 and 6.96 μg/kg, respectively.
建立并验证了一种基于超高效液相色谱的方法，用于检测牛粪便中的六种甲状腺抑制剂化合物：他巴唑、丙基硫氧嘧啶、甲巯咪唑、甲基硫氧嘧啶、苯丙噻唑和硫脲。甲状腺抑制剂用甲醇和缓冲液（pH=8）的混合物从基质中提取。然后，用 3-碘苄基溴将分析物衍生化。衍生物的液相色谱分离在 SB-C18 柱（50×2.1mm；1.8μm，Agilent）上进行，使用乙腈/0.1%乙酸的流动相在 7.5 分钟内进行梯度洗脱。分析在 Shimadzu NEXERA X2 超高效液相色谱仪上进行，配备三重四极杆 MS 8050 仪器，以正电喷雾电离模式运行。根据目标化合物，监测两个或三个诊断信号（选择反应监测转换）。该程序是根据委员会决定 2002/657/EC 进行验证的。回收率和重复性符合本文件对禁用化合物规定的性能标准。回收率在 97.5%至 110.5%之间，重复性不超过 14.1%。决策限制和检测能力均低于 10μg/kg。苯基噻唑的决策限制和检测能力最高浓度分别为 3.48μg/kg 和 6.96μg/kg。
