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[使用超高效液相色谱-串联质谱法测定牛尿液中的甲状腺抑制剂]

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

作者信息

Lech Rodziewicz, Jolanta MasŁOwiecka, Anna Sadowska, Halina Car

机构信息

Laboratory of Chemical Examination of Foodstuffs, Department of Veterinary Hygiene, Bialystok 15-959, Poland.

Department of Experimental Pharmacology, Medical University of Bialystok, Bialystok 15-295, Poland.

出版信息

Se Pu. 2017 Oct 8;35(10):1048-1054. doi: 10.3724/SP.J.1123.2017.05004.

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 -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.

摘要

采用超高效液相色谱 - 串联质谱法(UHPLC - MS/MS)在正电喷雾电离模式下测定了牛尿中的五种甲状腺抑制剂(TSs),即他巴唑、硫脲、甲基硫脲、丙基硫脲和苯基硫脲。使用带有叔丁基甲基醚的ChemElut柱进行萃取和净化,无需衍生化步骤。在Acquity UPLC SS T3柱上实现分离。流动相为乙腈和含有0.2%(v/v)甲酸的水。质谱仪在多反应监测模式下运行。向尿液样品中加入浓度分别对应于5、10、15和20 μg/L的TS溶液。准确度(经内标校正)范围为92%至107%,所有五种分析物的重复性精密度(相对标准偏差,RSD)均小于15%。实验室内再现性的RSD小于26%。决策限(CCα)和检测能力(CCβ)从校准曲线获得,分别在3.1 - 6.1 μg/L和4.0 - 7.4 μg/L范围内。CCα和CCβ值低于设定为10 μg/L的推荐浓度。结果表明,所描述的方法适用于直接检测牛尿中的TSs。该方法也可用于测定猪尿中的TSs。

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