摘要
目的建立LC-MS/MS法测定人血浆中氯沙坦及其代谢物E-3174血药浓度的方法。方法血浆酸化后用乙醚提取,采用同位素内标(氘3-E-3174)进行测定。色谱柱:CAPCELL PACK C_(18)Ⅲ(100mm×2.0mm,5μm),流动相:0.02%甲酸乙腈-水溶液(53:47,V/V);等度洗脱;流速0.3mL·min^(-1);进样体积5μL;电喷雾离子化,正离子MRM扫描。结果氯沙坦和E-3174线性范围均为5～500μg·L^(-1)(r>0.999),最低定量限均为5μg·L^(-1),平均提取回收率均>50%,批内、批间精密度RSD均<8%。结论本方法灵敏度高、专一性好、操作简单,适用于氯沙坦的药动学研究。
AIM To develop a LC-MS/MS method for the determination of losartan and its active metabolite E- 3174 in human plasma. METHODS The plasma samples were extracted with ethyl ether after acidification and isotope-labeled internal standards （Losartan-d3 carboxylic acid, IS） was used. The analytical column was CAPCELL PACK C18 Ⅲ （100 mm×2.0 mm,5 μm）. The mobile phase consisted of 0.02% formic acid acetonitrile and water（53：47, V/V）, and the flow rate was 0.3 mL·min-1. The injection volume was 5μL. The protonated ions of analytes were detected in positive ionization by multiple reaction monitoring （MRM） mode. RESULTS The assay was vahdated from 5 to 500 μg·L-1（ r 〉 0.999）in plasma for losartan and E-3174. The lower lirrdt of quantitation was both 5 μg·L-1 The extraction recovery was more than 50%. The intra- and inter-batch precisions （RSD） were all less than 8%. CONCLUSION The established LC-MS/MS method is shown to be sensitive, accurate, simple and suitable for the pharmacokinetic research of losartan.
出处
《中国临床药学杂志》
CAS
2010年第6期342-346,共5页
Chinese Journal of Clinical Pharmacy
基金
上海市科委科研计划项目(编号:08411966700)
