Drug Clinical Trial Institution, Wuxi People' Hospital, Nanjing Medical University, Wuxi 214023, China.
Drug Clinical Trial Institution, Wuxi People' Hospital, Nanjing Medical University, Wuxi 214023, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Apr 15;957:36-40. doi: 10.1016/j.jchromb.2014.03.004. Epub 2014 Mar 12.
A high-performance liquid chromatographic-tandem mass spectrometric (HPLC-MS/MS) method was developed and validated to determine sitafloxacin in human plasma with dextrorphan as internal standard. Chromatographic separation was performed on a ZORBAX SB-C18 column (3.5μm, 2.1mm×100mm) with the mobile phase of methanol/water (containing 0.1% formic acid) (46:54, v/v) at a flow rate of 0.2mL/min. Quantification was performed using multiple-reaction monitoring of the transitions at m/z 410.2 → 392.2 for sitafloxacin and m/z 258.1 → 157.1 for dextrorphan, respectively. The calibration curve was linear over the range of 5-2500ng/mL with the lower limit of quantification of 5ng/mL for sitafloxacin. The intra- and inter-day precisions were less than 8.3% and the deviations of assay accuracies were within ±4.1%. Sitafloxacin was sufficiently stable under all relevant analytical conditions. This method was successfully applied to the pharmacokinetic study of sitafloxacin in healthy Chinese volunteers.
建立并验证了一种高效液相色谱-串联质谱法（HPLC-MS/MS），用于测定人血浆中的司他沙星，以内标右啡烷为定量分析物。采用 ZORBAX SB-C18 柱（3.5μm，2.1mm×100mm），以甲醇/水（含 0.1%甲酸）（46:54，v/v）为流动相，流速为 0.2mL/min，实现色谱分离。司他沙星和内标右啡烷的检测分别采用 m/z 410.2→392.2 和 m/z 258.1→157.1 的多重反应监测模式进行定量分析。司他沙星在 5-2500ng/mL 浓度范围内线性良好，定量下限为 5ng/mL。日内和日间精密度均小于 8.3%，测定准确度的偏差在±4.1%范围内。司他沙星在所有相关分析条件下均稳定。该方法成功应用于健康中国志愿者的司他沙星药代动力学研究。
