Gowda K Veeran, Mandal Uttam, Senthamil Selvan P, Sam Solomon W D, Ghosh Animesh, Sarkar Amlan Kanti, Agarwal Sangita, Nageswar Rao T, Pal Tapan Kumar
Bioequivalence Study Centre, Department of Pharmaceutical Technology, Jadavpur University, Kolkata, India.
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Oct 15;858(1-2):13-21. doi: 10.1016/j.jchromb.2007.07.047. Epub 2007 Aug 10.
A simple, rapid, sensitive and specific liquid chromatography-tandem mass spectrometry method was developed and validated for quantification of metoprolol tartrate (MT) and ramipril, in human plasma. Both the drugs were extracted by liquid-liquid extraction with diethyl ether-dichloromethane (70:30, v/v). The chromatographic separation was performed on a reversed-phase C8 column with a mobile phase of 10 mM ammonium formate-methanol (3:97, v/v). The protonated analyte was quantitated in positive ionization by multiple reaction monitoring with a mass spectrometer. The method was validated over the concentration range of 5-500 ng/ml for metoprolol and ramipril in human plasma. The precursor to product ion transitions of m/z 268.0-103.10 and m/z 417.20-117.20 were used to measure metoprolol and ramipril, respectively.
建立并验证了一种简单、快速、灵敏且特异的液相色谱-串联质谱法,用于定量测定人血浆中的酒石酸美托洛尔(MT)和雷米普利。两种药物均通过用乙醚-二氯甲烷(70:30,v/v)进行液-液萃取来提取。色谱分离在反相C8柱上进行,流动相为10 mM甲酸铵-甲醇(3:97,v/v)。通过质谱仪在正离子模式下采用多反应监测对质子化分析物进行定量。该方法在人血浆中酒石酸美托洛尔和雷米普利的浓度范围为5-500 ng/ml内进行了验证。分别使用m/z 268.0-103.10和m/z 417.20-117.20的前体离子到产物离子的跃迁来测定酒石酸美托洛尔和雷米普利。