Citation: Lech RODZIEWICZ, Jolanta MASŁOWIECKA, Anna SADOWSKA, Halina CAR. Determination of thyreostats in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2017, 35(10): 1048-1054. doi: 10.3724/SP.J.1123.2017.05004 shu

Determination of thyreostats in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry

1.
Laboratory of Chemical Examination of Foodstuffs, Department of Veterinary Hygiene, Bialystok 15-959, Poland;
2.
Department of Experimental Pharmacology, Medical University of Bialystok, Bialystok 15-295, Poland

Received Date: 5 May 2017

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 μg/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 (CCα) and detection capabilities (CCβ) were obtained from a calibration curve and were in the ranges of 3.1-6.1 μg/L and 4.0-7.4 μg/L, respectively. The CCα and CCβ values were below the recommended concentration, which was set at 10 μg/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.
- ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS),
- thyreostats (TSs),
- urine
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1.
沈阳化工大学材料科学与工程学院沈阳 110142