摘要
目的建立比格犬血浆中氨氯地平的HPLC-MS/MS定量测定方法。方法 HPLC分离采用Zorbax SB-C18柱,流动相为乙腈-水(42∶58,0.1%甲酸,4 mmol·L-1醋酸铵),流速为0.2 ml·min-1;质谱检测采用电喷雾(ESI)离子源,正离子多反应监测(MRM)方式检测。血浆样品经甲醇-乙腈混合液沉淀蛋白、高速离心后进样分析,检测反应为m/z409.4-238.1(氨氯地平),m/z256.2-167.0(苯海拉明,内标)。结果氨氯地平在比格犬血浆中定量范围为0.5~500 ng·ml-1,日内和日间精密度≤9.04%、回收率高且血浆样品稳定性好。结论本方法特异、快速、准确、可靠,可满足氨氯地平比格犬血浆动力学研究需要。
Objective To develop an HPLC-MS/MS method for the quantification of amlodipine in plasma of Beagle dogs. Methods Amlodipine and diphenhydamine (internal standard, IS) were separated on a Zorbax SB- C18 column (2.1 mm x50 ram,3.5 txm) with a mobile phase of acetonitrile-water (42: 58) containing 0.1% for- mic acid and 4 mmol .L-1 ammonia acetate at a flow rate of 0.2 ml .min -1. The plasma sample was prepared by a simple deproteinization with methonal-acetonitrile ( 1 : 2) followed by centrifugation. Detection was performed in a positive multiple reaction monitoring(MRM) mode with an electrospray ionization (ESI) source. The reaction moni- tored was m/z 409.4-238.1 for amlodipine and m/z 256.2-167.0 for diphenhydamine (IS). Results The quantifica- tion range for amlodipine in Beagle dog plasma was 0.5-500 ng .m1-1. The intra- and inter-day precision(RSD) was no more than 9.04 % with a high recovery and good stability for quantification. Conclusion This method is spe- cific, quick, accurate and reliable for the pharmacokinetic study of amlodipine in Beagle dogs.
出处
《解放军药学学报》
CAS
2013年第2期97-100,共4页
Pharmaceutical Journal of Chinese People's Liberation Army
基金
国家科技重大专项课题
No.2012ZX09301002-001-007