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

作　　者：Lech RODZIEWICZ Jolanta MASLOWIECKA Anna SADOWSKA Halina CAR 

机构地区：[1]Laboratory of Chemical Examination of Foodstuffs,Department of Veterinary Hygiene [2]Department of Experimental Pharmacology,Medical University of Bialystok

出　　处：《色谱》2017年第10期1048-1054,共7页Chinese Journal of Chromatography

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 20μg/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 3.1-6.1μg/L and 4.0-7.4μg/L,respectively.The CCαand CCβvalues were below the recommended concentration,which was set at 10μg/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.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.

关 键 词：ultra-high performance liquid chromatography-tandem mass SPECTROMETRY (UHPLC-MS/MS) thyreostats (TSs) URINE 

分 类 号：O658[理学—分析化学]