一种用于生物样品中环丙沙星的改进高效液相色谱分析法。

An improved HPLC assay for ciprofloxacin in biological samples.

作者信息

Pei Y Y, Meng X, Nightingale C H

机构信息

School of Pharmacy, University of Connecticut, Storrs 06268.

出版信息

Zhongguo Yao Li Xue Bao. 1994 May;15(3):197-201.

PMID:7976369

Abstract

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 Nucleosil C18 (4.6 mm x 250 mm) using fluorescence detection with lambda exc 274 nm and lambda emi 418 nm. The mobile phase was composed of acetonitrile 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 > or = 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.

摘要

建立了一种简单、灵敏的高效液相色谱法，用于测定0.1 ml兔、人血清及脑脊液中的环丙沙星（Cip）。采用Nucleosil C18（4.6 mm×250 mm）色谱柱，以乙腈和含5 mmol·L⁻¹硫酸氢四丁铵的10 mmol·L⁻¹磷酸盐缓冲液（pH 2.7，体积比18:82）为流动相，流速为1.0 ml·min⁻¹，在激发波长274 nm、发射波长418 nm下进行荧光检测，实现了Cip与吡哌酸（内标）的分离。Cip的保留时间为5.9 min，吡哌酸的保留时间为4.0 min。日间变异系数<6.97%（n = 5），日内变异系数<3.33%（n = 5）。血清检测限为3 ng·ml⁻¹，脑脊液检测限为5 ng·ml⁻¹（r≥0.9996）。以0.33、1.0和2.5 mg·kg⁻¹·h⁻¹的恒定速率静脉输注期间，同时测定兔血清和脑脊液中Cip的浓度-时间曲线，证明了该方法的应用。