LC-MS/MS测定患者血浆中莫西沙星的浓度

Determination of Moxifloxacin in Patients Plasma by LC-MS/MS

关键词:  莫西沙星  液质联用法  血药浓度

Key words:  moxifloxacin  LC-MS/MS  plasma drug concentration

摘要:

目的 采用LC-MS/MS测定患者血浆中莫西沙星浓度，并进行血药浓度监测。方法 血浆样品用乙腈沉淀蛋白后，以普瑞巴林为内标，选用ZORBAX SB C₁₈（2.1 mm×100 mm，3.5 μm）色谱柱，以乙腈-水（均含0.1%甲酸）为流动相梯度洗脱，流速为0.30 mL·min^-1，柱温为30℃，进样量为10 μL，总分析时间为4.0 min；采用电喷雾离子化源，正离子方式，多反应监测扫描方式进行监测。结果 血浆中莫西沙星浓度线性范围为10~5 000 μg·mL^-1（r=0.997 8），定量下限为10 ng·mL^-1；质控样品准确度为94.2%~107.1%；日内、日间RSD<15%；样品和内标提取回收率在82.4%~89.8%。结论 该方法快速、灵敏、准确，专属性强，重复性好，适用于莫西沙星临床血药浓度测定。

Abstract:

OBJECTIVE To develop an LC-MS/MS method for determination of moxifloxacin in patients plasma and applied to drug monitoring. METHODS The plasma samples were precipitated with acetonitrile, with pregabalin as an internal standard. The separation was achieved on ZORBAX SB C₁₈column (2.1 mm×100 mm, 3.5 μm) and eluted with linear gradient using acetonitrile and water (both contain 0.1% formic acid) at the flow rate of 0.30 mL·min^-1, the injection volume was 10 μL and the column temperature was 30℃. The total time of the analysis was 4.0 min. Detection of the analytes were achieved using positive ion electrospray ionization (ESI) in the multiple reaction monitoring (MRM) mode. RESULTS The linear calibration curve of moxifloxacin obtained concentration range of 10-5 000 ng·mL^-1(r=0.997 8), with the lower limit of quantitation (LLOQ) of 10 ng·mL^-1. The accuracy of quality control sample was 94.2%-107.1%. Intra-day and inter-day relative standard deviations were both <15%. The extraction recovery of low, middle and high concentrations was 82.4%-89.8%, respectively. CONCLUSION The established method is rapid, sensitive, accurate, specific and reliable, and it is suitable for the study of therapeutic drug monitoring of moxifloxacin.