HPLC法快速测定吉米沙星尿药浓度及其尿排泄研究

Rapid Determination of Gemifloxacin in Urine by HPLC and Study on Excretion of It by Urine

目的：建立快速测定人尿液中吉米沙星药物浓度的方法，并考察其尿排泄情况。方法：尿样用甲醇处理后以高效液相色谱法测定，色谱柱为KromasilC18,流动相为乙腈．10mmol／L醋酸铵缓冲液（pH2．2，含10mmoUL高氯酸）（22：78，玎矿），柱温为40℃，流速为1．5ml／min，检测波长为338nm。结果：吉米沙星尿药浓度在O．1～100μg／ml范围内线性关系良好（r=0．9993），最低检测质量浓度为0．05μg／ml；平均方法回收率为93．0％～102．7％，平均提取回收率为103．2％～109．4％，日内RSD为1．3％～5．7％，日间RsD为5．3％～9．5％。国产及进口吉米沙星片48h尿累积排泄率分别为（37．4±7．5）％和（41．2±14．0）％。结论：本方法简便、快速、灵敏、重现性好，适用于吉米沙星尿药浓度测定。

OBJECTIVE： To establish a method for rapid determination of gemifloxacin in human urine and to investigate the excretion of gemifloxacin by urine. METHODS： HPLC method was adopted to detect urine sample after treated with methanol. The determination was performed on Kromasil C18 column with mobile phase consisted of acetonitrile-10 mmol/L ammonium acetate buf- fer（pH 2.2, containing 10 mmol/L perchloric acid, 22：78, V/V） at flow rate of 1.5 ml/min. The column temperature was 40 ℃, and detection wavelength was set at 338 nm. RESULTS： The linear range of gemifloxacin in urine were 0.1-100 μg/mL （r=0.999 3） ; the lowest detection limit was 0.05 μg/ml with average method recoveries of 93.0%-102.7% and extraction recoveries of 103.2%-109.4% ; RSD of intra-day and inter-day were 1.3%-5.7% and 5.3%-9.5%, respectively. Accumulative excretion rates of domestic and imported Gemifloxacin tablet by urine within 48 h were （37.4± 7.5）% and （41.2 ±14.0）%, respectively. CONCLU- SIONS ： The method is found to be convenient, rapid, sensitive and reproducible for the determination of gemifloxacin in urine.