摘要
目的 建立LC-MS-MS法测定人血浆中雷米普利及其活性代谢产物雷米普利拉的浓度.方法 以依那普利为内标,采用甲醇-0.1%甲酸溶液(75∶25)为流动相,以Waters Atlantis C18色谱柱为分析柱,通过电喷雾电离源(ESI),以选择离子反应监测(SRM)方式进行检测.用于定量分析的离子反应分别为m/z 417.3→234.3(雷米普利)、m/z 389.3→206.2(雷米普利拉)和m/z 377.3→234.2(依那普利).结果 雷米普利和雷米普利拉分别在0.103~102.7 ng·mL-1和0.106~106.4 ng·mL^-1浓度范围内线性良好.最低检测限分别为0.05 ng·mL^-1和0.10 ng·mL^-1(S/N=5).雷米普利和雷米普利拉的日内、日间精密度(RSD)均小于9%,低、中、高3个浓度的方法回收率均大于90%.结论 本法专属性强,样品处理方便,灵敏度高,适用于雷米普利临床药物动力学研究.
OBJECTIVE To establish a LC-MS-MS method for the determination of ramiprilat and its active metabolite ramiprilat in the human plasma. METHODS Enalapril was used as the internal standard. Ramipril and Ramiprilat was chromatographed by using a Waters Atlantis C18 column. The mobile phase consisted of metanol- 0. 1% formic acid solution(75:25 ). Electrospray ionization (ESI) source was applied and operated in the positivion mode. Selected reaction monitoring(SRM) mode with the transitions of m/z 417.3→234.3 ,m/z 389.3→206.2 and m/z 377.3→234.2 were used to quantify ramipril,ramiprilat and the internal standard, respectively. RESULTS The assay linearities of ramipril and ramiprilat were confirmed over the range 0. 103 - 102.7 ng · mL^-1 and 0. 106 - 106.4 ng · mL^-1 , and their detect limits of were 0.05 ng · mL^-1and 0. 10 ng· mL^-1 , respectively. The inter and intra-day precision (RSD) were less than 9% . The average recoveries were above 90%. CONCLUSION The method was proved to be robust, covenient, sensitivity and suitable for the clinical investigation of ramipril pharmacokinetics.
出处
《中国现代应用药学》
CAS
CSCD
北大核心
2007年第4期310-313,共4页
Chinese Journal of Modern Applied Pharmacy