高效液相色谱法测定人子宫、输卵管及血清中氧氟沙星浓度

DETERMINATION OF OFLOXACIN IN HUMAN FALLOPIAN TUBE,UTERUS AND SERUM BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

目的 建立人组织及血清中氧氟沙星含量的HPLC测定方法。方法 采用HypersilC1 8柱分离 ,流动相为乙腈 0 0 1moL·L- 1 磷酸盐缓冲液 0 5moL·L- 1 四丁基溴化铵 (9∶91∶4 ,pH 2 5 ) ,流速 1 0mL·min- 1 ,在UV 2 94nm处测定 ;样品经匀浆或用液氮冷冻研磨至粉末状 ,用 1%曲拉通 10 0溶解 ,乙酸乙酯 异丙醇 (9∶1)提取 ,HPLC测定。结果氧氟沙星浓度在 0 2～ 8 0 μg·mL- 1 与峰高比呈线性关系 ,最小检测限 4 0ng·mL- 1 ,用本法对 2 0例妇产科病人进行药物浓度测定 ,取得了满意的结果。结论 此方法适用于人体组织中氧氟沙星浓度的测定 。

AIM To establish a method for determineation of the concentration of ofloxacin in human fallopian tube, uterus and serum. METHODS The separation was performed on a Spherisob C 18 column (Hypersil, 250 mm×4 6 mm ID, 5 μm) with a mobile phase of acetonitrile 0 01 moL·L -1 potassium dihydrogen phosphate 0 5 mol·L -1 tetrabutylammonium bromide (9∶91∶4, pH 2 5). The flow rate was 1 0 mL·min -1 and detection was at 294 nm. The samples were homogenated or ground to powder after freezing with liquid nitrogen. 1%triton 100 and certain volume of ethylacetate isopropanol (10∶1) were added, shaken and centrifuged. Then the entire organic layer was transferred to a tube and vacuum dried. The residue was reconstituted in the mobile phase for HPLC. RESULTS There was a linear relationship between the peak area ratio and the ofloxacin concentration over the range of 0 2～8 0 μg·mL -1 . The limits of detection was 40 ng·mL -1 . Using this method to determine the ofloxacin concentrations in relevant organs as well as in the plasma of patients of the Department of Gynecology, and achieved satisfactary results. CONCLUSION The method can be applied to assay the ofloxacin concentration in human tissues. Ofloxacin was well distributed in woman fallopian tube, uterus and serum after single oral adminstration.