液相色谱-质谱串联法测定人血浆头孢卡品浓度

Determination of Cefcapene in Human Plasma By LC-MS/MS

目的建立测定人血浆头孢卡品浓度的液相色谱-质谱串联方法。方法血浆样品经甲醇沉淀蛋白,以甲醇∶2.5 mmol.L-1醋酸铵缓冲液(32∶68)为流动相,Waters Symmetry C18(3.9 mm×150 mm,5μm)色谱柱分离,样本经电喷雾离子源负离子化,通过三重四极杆串联质谱仪,在多反应监测模式下对头孢卡品(m/z452.1→348.1)和内标头孢拉定(m/z409.1→270.0)的浓度进行测定。结果血浆头孢卡品在3.600～3 600μg.L-1范围内线性良好,定量下限3.600μg.L-1,批内精密度<4.3%,批间精密度<2.1%,提取回收率为97.0%～102.5%。结论该分析方法简便、灵敏、准确,适用于盐酸头孢卡品酯片人体药动学研究。

Objective To establish a method for determinating cefcapene by LC-MS/MS.Methods The plasma samples were precipitated for protein with methanol.Methanol-2.5 mmoL·L-1 ammonium acetate（32：68） were used as mobile phase.The analysis was performed on Waters Symmetry C18 column（3.9 nm×150 mm,5 μm）.The samples were measured by a triple-quadrupole mass spectrometer in negative electron spray ionization（ESI） mode using multiple reaction monitoring（MRM）.The extracted ions monitored following MRM transitions were m/z 452.1→348.1 for cefcapene and m/z 409.1→270.0 for the internal standard cefradine.Results The calibration curve of cefcapene in human plasma was in linear relationship over the concentration rang of（3.600-3 600） μg·L-1.The lower limit of quantitation was 3.600 μg·L-1.The RSD of intra-day was less than 4.3%.The RSD of inter-day was less than 2.1%.The recovery was 97.0%-102.5%.Conclusion The method is proved to be convenient,sensitive and accurate,which can be used to study the pharmacokinetics of cefcapene pivoxil hydrochloride tablets in healthy volunteers.