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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 a high performance liquid chromatography tandem mass spectrometry (LC-MS / MS) for the simultaneous determination of isoniazid and moxifloxacin in human plasma and pleural effusion. Methods Theophylline was used as internal standard, plasma samples and pleural fluid samples were detected by acetonitrile precipitation protein. An Agilent ZORBAX SB-Aq column (4.6 mm × 150 mm, 5 μm) was used as the analytical column. Aqueous acetonitrile-5 mmol·L -1 ammonium acetate solution (containing 0.1% formic acid) ESI) was detected by positive ion multi-reaction monitoring (MRM). Isoniazid m / z 138.1 → 121.1, moxifloxacin m / z 402.1 → 384.0, theophylline m / z 181.1 → 124.0. Results The endogenous substances in plasma and pleural effusion had no interference with the determination. The linear range of isoniazid and moxifloxacin in plasma and pleural effusion were 0.1 ~ 10μg · mL -1, intra-day and inter-day precision (RSD) Less than 7.56%. Conclusion The method is specific, sensitive and reliable. It is suitable for high-throughput analysis of clinical plasma and pleural effusion samples.