液相色谱测定水样中的氧氟沙星手性对映体

Analysis of ofloxacin enantiomers in sewage by high performance liquid chromatography

利用大赛路(CHIRALCELOD-H)手性柱对氧氟沙星对映体进行分离,考察了在流动相组分、流动相添加剂和流速对手性分离的影响。结果表明,V正己烷∶V乙醇∶V乙酸=80∶20∶0.5的流动相能够使氧氟沙星得到较好的分离,左氧氟沙星和右氧氟沙星的质量浓度在0.25～5.00μg/mL范围内线性关系良好(r2=0.9997)。实际水样中该方法的最低检出限左氧氟沙星为0.28μg/L、右氧氟沙星为0.10μg/L,最低定量限左氧氟沙星为0.36μg/L、右氧氟沙星为0.21μg/L。氧氟沙星的两组浓度加标平均回收率左氧氟沙星90.1%和88.6%、右氧氟沙星为87.6%和85.4%,左氧氟沙星的相对标准偏差(RSD)为5.2%、6.4%,右氧氟沙星的RSD为4.8%、7.6%(n=3)。

A comprehensive method has been developed for the analysis of ofloxacin enantiomers in sewage by high performance liquid chromatography coupled with a fluorescence detector. Chiral separation was performed on a CHIRALCEL OD-H column using n-hexane-ethanol-acetic acid as mobile phase at a flow rate of 1.0 mL/min. The ofloxacin enantiomers were extracted by a weak cation ion exchange resin （WCX） and eluted with methanol, resulting in ofloxacin recoveries generally above 85 %. Good linearities were achieved in the range of 0.25 - 5.00μg/mL for R-ofloxacin and S-ofloxacin （ r^2 = 0. 9997）. The limits of quantitation （LOQ） were estimated to be about 0.36 μg/L for S-ofloxacin and 0.21μg/mL for R-ofloxacin. An actual sample was determined quantitatively using the above method.