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液质联用检测大鼠血、尿液和胆汁中氯沙坦的含量
蒋华芳1,2,段明郁2,邢金松2,赵宁2,AgelaWong2,范国荣1*
0
(1.第二军医大学药学院药物分析学教研室,上海 200433*2.上海药明康德新药开发有限公司,上海 200131)
摘要:
目的:建立LC/MS/MS法测定大鼠血﹑尿液和胆汁中氯沙坦的浓度,研究氯沙坦在大鼠体内的药物动力学特点。方法:大鼠血浆样品采用沉淀蛋白作为前处理方法,尿液和胆汁采用液-液萃取方法进行前处理,进样检测。色谱柱为Agela Venusil MP-C18 2.1 mm×50 mm,粒径5 μm;流动相A为0.1%甲酸,流动相B为0.1%甲酸(溶剂为乙腈)。采用梯度洗脱:流动相B在1.5 min内从20%到95%,流速0.35 ml/min,进样量为10 μl,质谱仪检测,离子源为ESI源。结果:氯沙坦在血、尿液和胆汁中的线性范围为1~1 000 μg/L,线性良好(r>0.99),平均相对回收率>80.0%,日内和日间精密度均小于15%。结论:该检测方法操作方便,结果准确,专属性强,可用于血﹑尿液和胆汁中氯沙坦药物含量的测定。
关键词:  氯沙坦  血浆  胆汁  尿  液质联用
DOI:10.3724/SP.J.1008.2008.01091
投稿时间:2008-02-20修订日期:2008-06-16
基金项目:
Determination of losartan concentrations in rat plasma,urine and bile by liquid chromatography-tandem mass spectrometry
JIANG Hua-fang1,2,DUAN Ming-yu2,XING Jin-song2,ZHAO Ning2,Agela Wong2,FAN Guo-rong1*
(1.Department of Drug Analysis,School of Pharmacy,Second Military Medical University,Shanghai 200433,China*2.WuXi PharmaTech Co.,LTD,Shanghai 200131)
Abstract:
Objective:To establish a liquid chromatography-tandem mass spectrometry (LC/MS/MS) method for determination of the losartan concentrations in rat plasma,urine and bile.Methods: The method was based on a protein precipitation procedure for rat plasma and liquid-liquid extraction for rat urine and bile,then the diluted extract was analyzed by LC/MS/MS using turbo ion spray (TIS) positive ion mode.Chromatography was performed on an Agela Venusil MP-C18 column (5 μm particle,2.1 mm×50 mm) by gradient elution.Mobile phase A was 0.1% formic acid in water and mobile phase B was 0.1% formic acid in acetonitrile.The mobile phase B increased from 20% to 95% within 1.5 min,with the flow rate being 0.35 ml/min and the feeding rate being 10 μl.Electrospray ionization (ESI) ion source was used.Results: The linear range of losartan was 1-1 000 μg/L in the plasma,urine and bile of rats (r>0.99).The mean relative recovery rate was higher than 80.0%;RSD values of intra-day and inter-day were both less than 15%.Conclusion: The present method is easy to perform,accurate,and specific; it can be used for determination of losartan concentration in rat plasma,urine and bile.
Key words:  losartan  plasma  bile  urine  LC/MS/MS