摘要
目的建立HPLC-MS/MS法测定人血浆中米那普仑的质量浓度。方法用简单的蛋白沉淀法处理血浆,色谱柱:ZORBAX SB-Aq柱(2.1 mm×50 mm,3.5μm),流动相:甲醇-0.01%甲酸,梯度洗脱,流速:0.4 mL·min^(-1),柱温:20℃,用正离子扫描,多反应监测方式测定样品中药物的质量浓度。考察该方法的专属性、标准曲线与定量下限、精密度及回收率、基质效应和稳定性。结果血浆样品中,米那普仑在2.0~500.0 ng·mL^(-1)线性关系良好(r>0.999 8),定量下限为2.0 ng·mL^(-1)。血样日内与日间相对标准偏差(RSD)均小于15%,平均回收率>96%,且稳定性均较好。结论本方法简便快速、灵敏准确、特异性强,适用于测定人血浆中米那普仑的浓度。
Objective To develop a HPLC- MS / MS method for s determination of milnacipran in human plasma. Methods The plasma samples were prepared by protein precipitation. The separation was achieved on ZORBAX SB- Aq column（ 2. 1 mm × 50 mm,3. 5 μm）,eluted with a linear gradient using methanol -0. 01% formic acid at the flow rate of 0. 4 mL·min^-1. The column temperature was 30 ℃. Detection of the analyte was achieved by positive ion electrospray ionization in the multiple reaction monitoring（ MRM） mode. The specificity,lower limit of quantitation and standard curve,precision and recovery rate and stability as well as the matrix effect were investigated. Results The concentration of milnacipran was ranged from 20. 0 to 5 00. 0 ng ·mL^-1（ r〉0. 999 8）,with the lower limit of quantitation of 2. 0 ng · mL^-1. Intra- day and inter- day relative standard deviations（ RSD） were both below 15%.The recoveries of low,middle and high concentrations were 〉96%.Conclusion The method is simple,rapid,sensitive and accurate,specific,suitable for determination of milnacipran in human plasma.
出处
《中国临床药理学杂志》
CAS
CSCD
北大核心
2016年第7期643-645,共3页
The Chinese Journal of Clinical Pharmacology
