双手性选择剂毛细管电泳法分离分析氧氟沙星对映体
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摘要
建立了双手性选择剂毛细管电泳法分离分析氧氟沙星对映体。考察了环糊精种类及浓度、金属离子与手性配体的摩尔比、金属离子的浓度、背景电解质溶液的pH以及分离电压等因素对手性分离影响。在缓冲溶液为5 mmol/L磷酸二氢钠(含8 mg/mL羧甲基-β-环糊精,8 mmol/L Cu(II); Cu(II)与L-组氨酸的摩尔比为1:1. 3; pH 5. 0),分离电压为15 kV的优化条件下,氧氟沙星在15 min内达到基线分离,分离度为3. 44。并通过紫外分光光度法对其拆分机理进行了探讨。在最优电泳条件下,对左氧氟沙星中右氧氟沙星光学杂质的含量测定方法进行验证,右氧氟沙星的检测限和定量限分别为0. 5μg/mL和2μg/mL,在2～50μg/mL的浓度范围内线性关系良好(r~2=0. 9981),回收率为95. 0%～99. 5%,相对标准偏差为2. 3%～4. 0%。
A capillary electrophoresis method for the determination of ofloxacin enantiomers was established using a dual chiral selector system. The factors affecting its chiral separation including cyclodextrin species and concentration,molar ratio of metal ions to chiral ligands,concentration of metal ions,p H of background electrolyte solution and applied voltage were optimized. The best results were obtained by using 5 mmol/L sodium dihydrogen phosphate buffer( consisting of 8 mg/m L CM-beta-CD,8 mmol/L Cu( II),the ratio of Cu( II) to L-Histidine is 1: 1. 3,p H 5. 0),and voltage of 15 k V. The enantiomers of ofloxacin were baseline separated within 15 min with resolution of 3. 44. The separation mechanism was discussed by UV spectrophotometry. The optimal electrophoresis condition was extensively validated for the method of determination of the R-( +)-ofloxacin optical impurity in S-(-)-ofloxacin. The LOD and LOQ for the R-( +)-ofloxacin were 0. 5 and 2 μg/m L,respectively. A linear calibration curve was obtained in the concentration range of 2 ～ 50 μg/m L( r~2= 0. 9981). The recoveries were 95. 0% ～ 99. 5% with relative standard deviations of 2. 3% ～ 4. 0%.
A capillary electrophoresis method for the determination of ofloxacin enantiomers was established using a dual chiral selector system. The factors affecting its chiral separation including cyclodextrin species and concentration,molar ratio of metal ions to chiral ligands,concentration of metal ions,p H of background electrolyte solution and applied voltage were optimized. The best results were obtained by using 5 mmol/L sodium dihydrogen phosphate buffer( consisting of 8 mg/m L CM-beta-CD,8 mmol/L Cu( II),the ratio of Cu( II) to L-Histidine is 1: 1. 3,p H 5. 0),and voltage of 15 k V. The enantiomers of ofloxacin were baseline separated within 15 min with resolution of 3. 44. The separation mechanism was discussed by UV spectrophotometry. The optimal electrophoresis condition was extensively validated for the method of determination of the R-( +)-ofloxacin optical impurity in S-(-)-ofloxacin. The LOD and LOQ for the R-( +)-ofloxacin were 0. 5 and 2 μg/m L,respectively. A linear calibration curve was obtained in the concentration range of 2 ～ 50 μg/m L( r~2= 0. 9981). The recoveries were 95. 0% ～ 99. 5% with relative standard deviations of 2. 3% ～ 4. 0%.
引文
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