HPLC测定吉米沙星血药浓度

Determination of Gemifloxacin in Plasma by HPLC

关键词:  吉米沙星  血药浓度  高效液相色谱法

Key words:  gemifloxacin  plasma concentration  HPLC

摘要:

目的 建立高效液相色谱法快速测定人血浆中吉米沙星药物浓度。方法 色谱柱为Kromasil C₁₈(250 mm×4.6 mm，5 mm)；流动相为乙腈-10 mmol·L^-1醋酸铵缓冲液(pH 2.2，含10 mmol·L^-1高氯酸)(22∶78)；柱温40 ℃；流速1.5 mL·min^-1；检测波长为338 nm。血浆样品经5%硫酸锌甲醇溶液沉淀蛋白后进样测定。结果 本测定方法的线性范围：0.05~5 μg·mL^-1，r=0.999 9。方法回收率93.2%~104.8%，批内RSD为1.8%~5.1%，批间RSD为7.7%~8.5%。吉米沙星的最低检测浓度为0.02 μg·mL^-1。结论 本方法简单、快速、灵敏、重复性好，适用于吉米沙星生物利用度及人体药动学研究。

Abstract:

OBJECTIVE To establish a rapid HPLC method for determination of gemifloxacin in plasma. METHODS A Kromasil C₁₈ column(4.6 mm×250 mm, 5μm) was used at 40 ℃. Mobile phase was a mixture of CH3CN and 10 mmol·L^-1 ammonium acetate buffer (pH=2.2, containing 10 mmol·L^-1 perchloric acid) (22∶78). The flow rate was 1.5 mL·min^-1. The UV detector was operated at 338 nm. Plasma samples were treated by direct protein precipitation with 5% zinc sulfate-methanol solution. RESULTS The assay procedure was shown to produce linear calibration curves over the range of 0.05 μg·mL^-1 to 5 μg·mL^-1 of gemifloxacin in plasma(r=0.999 9). Within the range, the recovery rate was 93.2%-104.8%, and the RSD within-batch and between-batch were 1.8%~5.1% and 7.7%~8.5%, respectively. The detection limit of gemifloxacin was 0.02 μg·mL^-1. CONCLUSION This method is found to be reproducible, convenient and sensitive for bioavailability and clinical pharmacokinetics study of gemifloxacin.