LC-MS/MS同时测定人血浆及胸水中异烟肼和莫西沙星浓度

Determination of Isoniazid and Moxifloxacin in Human Plasma and Pleural Effusion by LC-MS/MS

目的建立高效液相色谱串联质谱(LC-MS/MS)同时测定人血浆及胸水中异烟肼和莫西沙星的浓度。方法以茶碱为内标,血浆样品及胸水样品经乙腈沉淀蛋白等处理后检测。采用Agilent ZORBAX SB-Aq(4.6 mm×150 mm,5μm)为分析柱;以乙腈-5 mmol·L^(-1)醋酸铵水溶液(含0.1%甲酸)为流动相,采用电喷雾离子源(ESI),以正离子多反应监测(MRM)方式进行检测,异烟肼m/z 138.1→121.1,莫西沙星m/z 402.1→384.0,茶碱m/z 181.1→124.0。结果血浆及胸水中内源性物质对测定无干扰,异烟肼和莫西沙星在血浆和胸水的线性范围均为0.1~10μg·mL^(-1),日内和日间精密度(RSD)均小于7.56%。结论本方法特异性强,灵敏度高,测定结果可靠,适用于临床血浆及胸水样品的高通量分析。

OBJECTIVE To establish an LC-MS/MS method for the determination of isoniazid and moxifloxacin in human plasma and pleura1 effusion. METHODS The theophylline was used as internal The protein of samples were precipitated with acetonitrile. The supernatant was separated on an Agilent ZORBAX SB-Aq （4. 6 mm × 150 mm, 5μm）. The mobile phase was consisted of acetonitrile and 5 mmol·L^-1 ammonium acetate（0. 1% formic acid solution）. Electrospray ionization （ESI） source was applied and operated in the positive multiple reaction monitoring （MRM） mode. The MS/MS ion transition of m/z was 138.1/121.1 for isoniazid, 402. 1→384. 0 for moxifloxacin and 181.1/124. 0 for theophylline. RESULTS Chromatograms showed no endogenous interfering peaks with blank samples. The calibration curves of isoniazid and moxifloxacin were both linear over the concentration range of 0. 1 - 10 -g·L^-1. Both inter-and intra-day relative standard deviations were less than 7.56%. CONCLUSION The method is specific, sensitive and accurate, and proved to be suitable for the determination of isoniazid and moxifloxacin in human plasma and pleural effusion samnles.