【摘要】 建立了动物尿液中氯噻嗪、氢氯噻嗪、氢氟噻嗪、氯噻酮、三氯噻嗪、甲氯噻嗪、呋噻米和依他尼酸等8种利尿剂残留检测的高效液相色谱-串联质谱(HPLC-MS/MS)方法。尿液样品经乙酸乙酯提取、阴离子交换固相萃取柱(PAX)净化、C18色谱柱分离、电喷雾离子化(ESI-)和选择反应监测(SRM)方式采集,外标法定量。该方法的检测限和定量限分别为10μg/L和20μg/L;利尿剂的测定在20~200μg/L范围内线性关系良好,相关系数R2大于0.99;猪尿在20、50和100μg/L三个添加浓度的平均回收率为74.0%~107.7%,批内RSD为5.2%~10.8%,批间RSD为5.7%~15.6%;牛尿在20、50和100μg/L三个添加浓度的平均回收率为71.1%~109.0%,批内RSD为3.9%~10.1%,批间RSD为6.4%~15.6%。更多还原

【Abstract】 A high performance liquid chromatography-tandem mass spectrometry method(HPLC-MS/MS) has been established for the determination of 8 diuretics residues in pig urine and bovine urine.The samples of urine were extracted by ethyl acetate,cleaned through PAX cartridges and separated through a C18 column.Mass spectrometry condition was electrospray ionization(ESI-) and selected reaction monitoring(SRM) mode.The quantification was carried out by the external standard method.The limit of detection(LOD) and quantification(LOQ) of the method were 10 μg/L and 20 μg/L respectively.The calibration curves have good linear within the range of 8 diuretics concentration from 20 μg/L to 200 μg/L,and the correlation coefficient was greater than 0.99.The average recoveries from spiked pig urine at three concentrations 20 μg/L,50 μg/L and 100 μg/L ranged from 74.0% to 107.7%,and the within-and between-run relative standard deviations(RSDs) were 5.2%～10.8% and 5.7%～15.6% respectively.The average recoveries from spiked bovine urine at the same three concentrations ranged from 71.1% to 109.0%,and the within-and between-run RSDs were 3.9%～10.1% and 6.4%～15.6% respectively.更多还原