论文部分内容阅读
目的:采用羧甲基-β-环糊精(CM-β-CD)为手性选择剂,建立测定氧氟沙星中对映体含量的毛细管电泳方法。方法:采用未涂层石英毛细管(50 cm×50μm,41 cm),在30 mmol·L-1的NaH2PO4缓冲溶液中加入(CM-β-CD)手性选择剂,调节不同的pH,分离电压为30 kV,得到优化的分离条件,在优化的分离条件下,对氧氟沙星对映体含量测定方法进行方法学验证,并采用该方法对3批样品进行检测。结果:在pH 4.0,30 mmol·L-1的NaH2PO4缓冲溶液,1.0%CM-β-CD,分离电压为30 kV条件下,左氧氟沙星和右氧氟沙星线性范围为0.025~0.200 mg·ml1(r=0.999 3和0.999 2),左氧氟沙星和右氧氟沙星的回收率分别为97.6%和97.8%,RSD分别为2.0和2.7%(n=9)。结论:羧甲基-β-环糊精对氧氟沙星有很高的对映体选择性,达到很好的分离效果。在不需要左、右氧氟沙星单纯对照品情况下,用于左氧氟沙星和右氧氟沙星的鉴别和含量测定。该方法重复性好,简便、快捷。
OBJECTIVE: To establish a capillary electrophoresis method for the determination of enantiomers in ofloxacin by using carboxymethyl-β-cyclodextrin (CM-β-CD) as chiral selector. Methods: CM-β-CD chiral selectors were added to 30 mmol·L -1 NaH 2 PO 4 buffer solution with uncoated quartz capillaries (50 cm × 50 μm, 41 cm) to adjust different pH and separate voltage Was 30 kV. The optimized separation conditions were obtained. The enantiomer content of ofloxacin was identified by methodology under optimized separation conditions. Three batches of samples were tested by this method. Results: The linear range of levofloxacin and of dexifloxacin was 0.025-0.200 mg · ml -1 (P <0.05) at pH 4.0 and 30 mmol·L -1 of NaH 2 PO 4 buffer, 1.0% CM-β-CD and the separation voltage was 30 kV r = 0.999 3 and 0.999 2). The recoveries of levofloxacin and of dexifloxacin were 97.6% and 97.8%, respectively, with RSDs of 2.0 and 2.7%, respectively (n = 9). Conclusion: Carboxymethyl-β-cyclodextrin has high enantioselectivity for ofloxacin and achieves good separation effect. In the absence of left and right ofloxacin simple reference substance case, for levofloxacin and dexufloxacin identification and determination. The method is repeatable, easy and fast.