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机构地区:[1]江南大学药学院,无锡214122 [2]江南大学食品科学与技术国家重点实验室,无锡214122 [3]江苏艾凡生物医药公司,无锡214122
出 处:《分析试验室》2014年第3期269-272,共4页Chinese Journal of Analysis Laboratory
基 金:国家自然科学基金(30972581);江苏省自然科学基金(BK2008110);江苏省兴卫工程平台项目(NO.ZX201108);2011年度江苏省双创计划(冯柏年)资助
摘 要:建立了高效液相色谱-串联质谱法测定兔血浆中吡喹酮浓度。血浆样品经乙腈沉淀蛋白,以WatersXBridgeC18柱(2.1×50mm,3.50ma)进行色谱分离,流动相为乙腈一体积分数0.1%甲酸溶液,梯度洗脱分离,三重四级杆质谱仪进行电喷雾离子化和正离子多离子反应监测模式检测吡喹酮。吡喹酮在0.8~2000.0ng/mL范围内线性关系良好,相关系数为0.9983,检出限为0.01ng/mL,在加样量为1600.0,160.0,2.5ng/mL的血浆样品中,吡喹酮的相对回收率为83.8%~104.8%,提取回收率为79.5%-96.5%,日内和日间RSD均小于6.4%。方法可用于吡喹酮血药浓度的测定。A high performance liquid chromatography-tandem mass (HPLC-MS/MS) method was developed for the determination of praziquantel in rabbit plasma. The plasma samples were pretreated using acetonitrile, separated by a Waters XBridge ClS column (2. 1 × 50 mm, 3.5μm)using the mobile phase composed of acetonitrile and 0. 1% formic acid solution with spectrometry using a Waters Quattro LC MicroMass a gradient elution program spectrometer in the positive and detected by tandem mass ion multiple reaction monitoring (MRM) scan mode with a electrospray ionization source. The linear range was 0. 8 - 2000. 0 ng/mL, the correlation coefficient was 0. 9983, and the quantification limit was 0. 01 ng/mL. At spiked levels of 1600. 0, 160.0,2.5 ng/mL in plasma, the relative recoveries of PZQ were 83.81% to 104.83%, the extraction recoveries were 79.51% to 96.50%, and the intra-and inter-day precisions were less than 6.4%. In conclusion, this method can be used for the determination of praziquantel in rabbit plasma.
关 键 词:吡喹酮 多离子反应监测 高效液相色谱-串联质谱法 血浆 浓度测定
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