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
建立了污水中26种痕量卡西酮类新精神活性物质的前处理及同时定量检测的方法,并成功应用于实际污水样品的检测。污水样品经过滤和加入内标溶液的预处理,在Oasis PRiME HLB固相萃取柱上经超纯水淋洗和甲醇溶液洗脱,在40℃下氮气吹干,用0...建立了污水中26种痕量卡西酮类新精神活性物质的前处理及同时定量检测的方法,并成功应用于实际污水样品的检测。污水样品经过滤和加入内标溶液的预处理,在Oasis PRiME HLB固相萃取柱上经超纯水淋洗和甲醇溶液洗脱,在40℃下氮气吹干,用0.1%甲酸-乙腈溶液(95∶5)复溶,利用高效液相色谱-串联质谱(high-performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)技术,采用选择反应监测(selected reaction monitoring,SRM)模式,用UPLC BEH C_(18)(100 mm×2.1 mm,1.7μm)色谱柱,柱温35℃,流动相为乙腈-0.1%甲酸的水溶液,梯度洗脱进行检测。经方法学验证,26种卡西酮类新精神活性物质的定量下限可达1.50~3.00 ng/L,其中21种待测物在1.50~375.0 ng/L范围内,5种在3.00~750.0 ng/L范围内,所有26种物质均具有良好的线性关系,相关系数r为0.99,批内和批间精密度的相对标准偏差(relative standard deviation,RSD)分别小于7.71%和13.91%,提取回收率均高于92.64%。该方法简单、准确、灵敏,可作为卡西酮类物质检测和滥用情况监测的方法。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.
