水产品中氧氟沙星对映体拆分研究  

Chiral Separation of Ofloxacin Enantiomers in Aquatic Products by High Performance Liquid Chromatography

作　　者：李维娜[1] 杨立业[1] 欧阳小琨[1] 王阳光[1] 

机构地区：[1]浙江海洋学院食品与药学学院,浙江舟山316004

出　　处：《浙江海洋学院学报（自然科学版）》2012年第6期513-517,共5页Journal of Zhejiang Ocean University(Natural Science Edition)

基　　金：国家自然科学基金(21276240);浙江省自然科学基金(Z3100533;Y2111223)

摘　　要：采用CHIRALCEL OD-H(4.6 mm×250 mm,5.0μm,Daicel)手性色谱柱拆分了氧氟沙星对映体,考察了流动相组成和流速等对手性分离的影响。确定了最佳的拆分条件:流动相为正己烷-乙醇(60:40,v/v),流速为0.6 mL/min,柱温为20℃,检测波长为294 nm。在此条件下氧氟沙星对映体的分离度为1.69。左氧氟沙星和右氧氟沙星的检出限分别为0.02μg/g和0.03μg/g,定量限分别为为0.04μg/g和0.05μg/g。左氧氟沙星平均回收率为83.46%,日间精密度和日内精密度的分别为0.34%和0.44%。右氧氟沙星平均回收率为87.32%。日间精密度和日内精密度分别为0.46%和0.69%。A high performance liquid chromatography method using the Chiralcel OD-H chiral column （4.6 min×250 mm, 5.0 Ixm, Daieel） for the chiral separation and determination of ofloxacin enantiomers was developed. The optimized chromatographic condition were hexane-ethanol （60：40, v/v） as the mobile phase with a flow rate of 0.6 mL/min and detection at the wavelength of 294 nm, the column temperature was set at 25 ℃ The resolution of ofloxacin enantiomers was 1.69 under the chromatographic conditions. The LOD of S-（-）- OFLX and R-（＋）-OFLX were 0.02 μg/g and 0.03μg/g, the LOQ of S-（-）OFLX and R-（＋）-OFLX were 0.04 μg/g and 0.05μg/g, respectively. The average recovery of S-（-） OFLX was 83.46%, the RSD of intra-day and inter-day preeisions were 0.34% and 0.44% respectively. The average recovery of R-（＋）-OFLX was 87.32%, the RSD of intra-day and inter-day precisions were 0.46% and 0.69% respectively.

关 键 词：高效液相色谱法 氧氟沙星 手性固定相 手性拆分 

分 类 号：O657.7[理学—分析化学]