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...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.展开更多
该文建立了快速测定畜肉中阿苯达唑及其代谢物(阿苯达唑砜、阿苯达唑亚砜、阿苯达唑-2-氨基砜)残留量的超高效液相色谱-串联质谱的分析方法。试样用乙腈提取,经QuEChERS试剂净化,通过Agilent ZORBAX Eclipse Plus C 18色谱柱分离,在正...该文建立了快速测定畜肉中阿苯达唑及其代谢物(阿苯达唑砜、阿苯达唑亚砜、阿苯达唑-2-氨基砜)残留量的超高效液相色谱-串联质谱的分析方法。试样用乙腈提取,经QuEChERS试剂净化,通过Agilent ZORBAX Eclipse Plus C 18色谱柱分离,在正离子多反应监测模式下分析,外标法定量。实验结果表明,阿苯达唑及其代谢物在各自的线性范围内线性关系良好(R ^(2)>0.998),检出限0.1~1μg/kg,在空白样品中进行3个浓度水平的添加实验,添加范围为0.1~10μg/kg,日内(n=6)平均回收率在81.9%~109.8%,日间(n=3)平均回收率在81.8%~99.0%,精密度为1.8%~14.4%。该方法操作简单、快速、准确、灵敏度高,重现性好,回收率高且稳定,检测限及定量限低于现有检测方法要求,可用于畜肉中阿苯达唑及其代谢物残留量的定性和定量分析。展开更多
文摘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.
文摘该文建立了快速测定畜肉中阿苯达唑及其代谢物(阿苯达唑砜、阿苯达唑亚砜、阿苯达唑-2-氨基砜)残留量的超高效液相色谱-串联质谱的分析方法。试样用乙腈提取,经QuEChERS试剂净化,通过Agilent ZORBAX Eclipse Plus C 18色谱柱分离,在正离子多反应监测模式下分析,外标法定量。实验结果表明,阿苯达唑及其代谢物在各自的线性范围内线性关系良好(R ^(2)>0.998),检出限0.1~1μg/kg,在空白样品中进行3个浓度水平的添加实验,添加范围为0.1~10μg/kg,日内(n=6)平均回收率在81.9%~109.8%,日间(n=3)平均回收率在81.8%~99.0%,精密度为1.8%~14.4%。该方法操作简单、快速、准确、灵敏度高,重现性好,回收率高且稳定,检测限及定量限低于现有检测方法要求,可用于畜肉中阿苯达唑及其代谢物残留量的定性和定量分析。
