色谱

色谱 ›› 2017, Vol. 35 ›› Issue (10): 1048-1054.DOI: 10.3724/SP.J.1123.2017.05004

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法测定牛尿液中的甲状腺抑制剂(英文)

Lech RODZIEWICZ1, Jolanta MASLOWIECKA1, Anna SADOWSKA2, Halina CAR2   

  1. 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
  • 收稿日期:2017-05-05 出版日期:2017-10-08 发布日期:2017-10-18
  • 通讯作者: Halina CAR,Tel:+48-85-7485554,E-mail:zfarmdosw@umb.edu.pl.

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

Lech RODZIEWICZ1, Jolanta MASLOWIECKA1, Anna SADOWSKA2, Halina CAR2   

  1. 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:2017-05-05 Online:2017-10-08 Published:2017-10-18

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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 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: thyreostats (TSs), ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), urine

Abstract:

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.

Key words: thyreostats (TSs), ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), urine

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