摘要
目的:建立同时测定犬血浆中依普利酮及其水解代谢物的液-质联用(LC-MS/MS)检测方法。方法:以同位素标记依普利酮为内标,血浆样品采用乙腈沉淀,色谱柱为Agilent TC-C18柱(2.1mm×50mm,5μm),流动相为乙腈-7.5mmol.L-1醋酸铵缓冲液(pH 7.0)(30∶70);流速0.2mL.min-1;依普利酮与其水解代谢物及内标分别选择m/z4 15.2→163.0,431.2→337.2,419.2→163.0。结果:依普利酮及其水解代谢物在5～2 000μg.L-1范围内线性良好,2组分平均提取回收率分别为80.17%与75.68%,日内和日间RSD均小于15%。结论:本方法灵敏度高,操作简便、快速,适用于依普利酮及其水解代谢物浓度测定。
OBJECTIVE To establish a sensitive and selective LC-MS/MS method for simultaneous determination of eplerenone and hydrolyzed eplerenone in beagle dog plasma. METHODS The plasma samples were precipitated by ice-cold acetonitrile with isotope labeling eplerenone as internal standard. Separation was achieved on an Agilent TC-C18 eversed-phase column （2. 1 mm×50 mm,5μm） with a mobile phase composed of acetonitrile-7. 5 mmol-L 1 ammonium acetate buffer （pH 7. 0） （30：70,v/v） at a flow rate of 0. 2 mE. min-1. The mass transition of m/z 415.2±163. 0,431.2→337. 2,and 419. 2→163.0 were used to detect eplerenone, hydrolyzed eplerenone and internal standard. RESULTS The assay was linear over the concen tration range 5 -2 000/~g＇L-I for eplerenone and hydrolyzed eplerenone in beagle dog plasma. Mean recoveries for eplerenone and hydrolyzed eplerenone at five concentration levels were 80. 17% and 75.68%. The method was accurate with all intra and inter day mean concentrations within 15% of nominal values at 5,10,500,1 500 and 2 000μg·L -1. CONCLUSION This meth-od was robust and suitable for concentration determination of eplerenone and hydrolyzed eplerenone.
出处
《中国医院药学杂志》
CAS
CSCD
北大核心
2010年第17期1454-1457,共4页
Chinese Journal of Hospital Pharmacy
