Liu X
Shanghai Institute for Drug Control, Shanghai 200233.
Yao Xue Xue Bao. 1998 Aug;33(8):600-4.
An analytical method for separation of ofloxacin enantiomers by HPCE using bovine serum albumin(BSA) as the chiral selector and isopropanol as the modifier was established. The effects of BSA concentration, pH of running buffer, isopropanol concentration, applied voltage and column temperature on the resolution of the enantiomers have been studied. The experimental results indicated that the BSA concentration and pH of the running buffer were the vital factors for the separation of the enantiomers. The concentration of isopropanol showed strong influence on the peak shape of enantiomers. Lower voltage and column temperature were favorable to improve the efficiency for the separation of the enantiomers. Optimum performance was achieved in a fused-silica capillary(45 cm x 30 microns ID, effective length 32 cm) at 30 degrees C and applied voltage of +15 kV with a pH 6.0 phosphate buffer containing 50 mg.ml-1 BSA and 5% isopropanol as running buffer and detected at 293 nm. The precision of this method was evaluated by repeated measurement of the migration times and peak areas for 0.45 mg.ml-1 ofloxacin standard solution. The RSD(n = 8) for migration times and peak areas were 1.6% and 1.1% for (-)-ofloxacin and were 1.8% and 2.8% for (+)-ofloxacin, respectively. The method was simple and fast and has been applied to separate enantiomers of ofloxacin products. The experimental results showed that the ratio of peak area of (-)-ofloxacin to that of (+)-ofloxacin was within the range of 0.995-0.998 with RSD(n = 6) of measurement between 1.8% and 2.0%.
建立了一种以牛血清白蛋白（BSA）为手性选择剂、异丙醇为改性剂，采用高效毛细管电泳法分离氧氟沙星对映体的分析方法。研究了BSA浓度、运行缓冲液pH值、异丙醇浓度、施加电压和柱温对映体分离度的影响。实验结果表明，BSA浓度和运行缓冲液pH值是对映体分离的关键因素。异丙醇浓度对映体峰形有较大影响。较低的电压和柱温有利于提高对映体的分离效率。在30℃、施加电压+15 kV的熔融石英毛细管（45 cm×30μm内径，有效长度32 cm）中，以含50 mg·ml-1 BSA和5%异丙醇的pH 6.0磷酸盐缓冲液为运行缓冲液，在293 nm处检测，可获得最佳性能。通过对0.45 mg·ml-1氧氟沙星标准溶液的迁移时间和峰面积进行重复测量，评价了该方法的精密度。（-）-氧氟沙星迁移时间和峰面积的RSD（n = 8）分别为1.6%和1.1%，（+）-氧氟沙星分别为1.8%和2.8%。该方法简便快速，已用于分离氧氟沙星产品的对映体。实验结果表明，（-）-氧氟沙星与（+）-氧氟沙星峰面积之比在0.995 - 0.998范围内，测量的RSD（n = 6）在1.8%至2.0%之间。
