作者:Lech; RODZIEWICZ; Jolanta; MASLOWIECKA...performanceliquidmassspectrometrythyreostatsurine
摘要:Five thyreostats (TSs) , namely tapazole, thiouracil, methylthiouracil, propylthiouracil, and phenylthiouracil,were determined in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) in positive electrospray ionization mode. Extraction and clean-up were achieved using a ChemElut cartridge with tert-butyl methyl ether, without a derivatization step. Separation was achieved on an Acquity UPLC SS T3 column. The mobile phase was acetonitrile and water containing 0.2% (v/v) formic acid. The mass spectrometer was operated in multiple reaction monitoring mode. Urine samples were spiked with TS solution at levels corresponding to 5, 10, 15, and 20 ug/L. The accuracy (internal standard corrected) ranged from 92% to 107%, with a repeatability precision (relative standard deviation,RSD) less than 15% for all five analytes. The RSDs within-laboratory reproducibility was less than 26%. The decision limits (CCa) and detection capabilities (CCp) were obtained from a calibration curve and were in the ranges of 3.1-6.1ug/L and 4.0-7.4ug/L, respectively. The CCa and CCp values were below the recommended concentration, which was set at 10ug/L .The results show that the described method is suitable for the direct detection of TSs in bovine urine. This method can also be used to determine TSs in porcine urine.
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