HPLC测定吉米沙星血药浓度

Determination of Gemifloxacin in Plasma by HPLC

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KromasilC18（250min×4．6mm，5μm）；流动相为乙腈-10mmol·L-1醋酸铵缓冲液（pH2．2，含10mmol·L-1高氯酸）（22：78）；柱温40℃；流速1．5mL·min^-1；检测波长为338nm。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：0．05-5μg·mL-1，r=0．9999。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0．02μg·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。

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 0.02μg·mL^-1. CONCLUSION This method is found to be reproducible, convenient and sensitive for bioavailability and clinical pharmacokinetics study of gemifloxacin.