改进的HPLC测定生物样品中环丙沙星浓度的微量分析法(英文)

An improved HPLC assay for ciprofloxacin in biological samples

介绍一种测定生物样品中环丙沙星(Cip)的HPLC方法及其应用实例。采用Nucleosil C_(18)为固定相,18:82乙腈一磷酸缓冲液10mmol·L^(-1)(含硫酸四丁基铵5mmol·L^(-1),pH 2.7)为流动相,荧光检测。本法对血清和脑脊液中Cip的最低检测浓度分别为3 ng·ml^(-1)和5 ng·ml^(-1),具有简便、灵敏、准确且样品需量少(0.1 ml)等优点。

A simple and sensitive high performance liquid chromatographic method was developed for determination of ciprofloxacin (Cip) in 0. 1 ml of rabbit and human serum and CSF. Separation of Cip and pipemidic acid (internal standard) was achieved on Nu-cleosil C28(4. 6 mm × 250 mm) using fluorescence detection with rexc 274 nm and remi 418 nm. The mobile phase was composed of ace-tonitrile and phosphate buffer 10 mmol · L-1 (pH 2. 7) containing tetrabutylammonium hydrogen sulfate 5 mmol · L-1(18 : 82, vol : vol) and the flow rate was set at 1.0 ml · min-1 The retention times were 5. 9 min for Cip and 4. 0 min for pipemidic acid. The inter-day coefficient of variation was <6. 97% (n = 5) and the intra-day coefficient of variation was < 3.33% (n = 5). The limits of detection were 3 ng · ml-1 serum and 5 ng · ml-1 CSF, (r> 0.9996). Application of this method was demonstrated with simultaneous measurements of concentration-time profiles of Cip in rabbit serum and CSF during iv infusions at constant rates of 0.33, 1.0, and 2. 5 mg · kg-1 · h-1.