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目的建立高效液相色谱质谱联用法测定西他沙星在人血浆中的浓度。方法色谱柱:Welch Ultimate C18(2.1 mm×50 mm,5μm);流动相:甲醇-水(0.1%甲酸水溶液);梯度洗脱;流速:0.4 mL·min~(-1)。用电喷雾离子化源,正离子,多反应检测模式进行扫描检测。西他沙星和非布司他的质荷比分别为m/z 410.1→392.1和m/z 317.1→261.1。考察该方法的专属性、标准曲线和定量下限、精密度与回收率、稳定性以及残留效应。结果血浆中西他沙星标准曲线线性范围为10~1500 ng·mL~(-1),最低定量下限为10 ng·mL~(- 1)。西他沙星的日内、日间精密度均小于15%,绝对回收率在76.18%~91.45%,残留为14.48%。在所有测试条件下西他沙星相当稳定。结论本方法快速、高效、灵敏,适用于血浆中西他沙星浓度的测定。
Objective To establish a HPLC-MS method for the determination of citaloxacin in human plasma. Methods Column: Welch Ultimate C18 (2.1 mm × 50 mm, 5 μm); mobile phase: methanol-water (0.1% formic acid aqueous solution); gradient elution; flow rate: 0.4 mL · min -1. Electrospray ionization source, positive ions, multi-reaction detection mode scan detection. The mass-to-charge ratios for xylofloxacin and febuxostat are m / z 410.1 → 392.1 and m / z 317.1 → 261.1, respectively. Investigate the specificity of this method, the standard curve and lower limit of quantitation, precision and recovery, stability and residual effects. Results The linear range of standard curve of sitaxacin in plasma was 10 ~ 1500 ng · mL -1 with the lowest limit of quantification being 10 ng · mL -1. The daily and intra-day precision of Sitafloxacin was less than 15%. The absolute recoveries ranged from 76.18% to 91.45% and the residuals were 14.48%. Sitaxir star is quite stable under all test conditions. Conclusion The method is rapid, efficient and sensitive and is suitable for the determination of the concentration of citalotoxin in plasma.