Wang Rong, Jia Zheng-Ping, Fan Jun-Jie, Hu Xiao-Li, Li Yong-Min, Chen Li-Ren, Xie Jing-Wen, Zhang Qiang
Department of Pharmacy, Lanzhou General Hospital, Lanzhou Command of PLA, Lanzhou, China.
Chirality. 2004 Jan;16(1):45-9. doi: 10.1002/chir.10305.
A capillary electrophoresis method was developed to separate the enantiomers of cefoperazone. Different cyclodextrins, including alpha-cyclodextrin (alpha-CD), beta-cyclodextrin (beta-CD), gamma-cyclodextrin (gamma-CD), 2-hydroxypropyl-beta-cyclodextrin (HP-beta-CD), and methyl-beta-cyclodextrin (Me-beta-CD), were tested as chiral additives in the running buffer. The effect of various parameters on enantioseparation such as concentration of NaH(2)PO(4), buffer pH, and CD concentration was also studied. The cefoperazone enantiomers were baseline separated under conditions of 0.04 mmol/L beta-CD, 75 mmol/L NaH(2)PO(4) buffer at pH 4.0. A fused silica capillary (40 cm effective length x 75 microm ID) was used. The applied voltage and capillary temperature were 20 kV and 25 degrees C, respectively. Under these conditions, linear calibration curves were obtained in the 5-500 microg/ml range using UV detection at 280 nm. The limit of detection for both isomers was 0.1 microg/ml. The method was used for the analysis of different pharmaceutical preparations (dose) and biological samples containing cefoperazone.
建立了一种毛细管电泳法分离头孢哌酮对映体。测试了不同的环糊精,包括α-环糊精(α-CD)、β-环糊精(β-CD)、γ-环糊精(γ-CD)、2-羟丙基-β-环糊精(HP-β-CD)和甲基-β-环糊精(Me-β-CD)作为运行缓冲液中的手性添加剂。还研究了各种参数如NaH(2)PO(4)浓度、缓冲液pH值和环糊精浓度对映体分离的影响。在0.04 mmol/L β-CD、pH 4.0的75 mmol/L NaH(2)PO(4)缓冲液条件下,头孢哌酮对映体实现了基线分离。使用了一根熔融石英毛细管(有效长度40 cm×内径75 μm)。施加电压和毛细管温度分别为20 kV和25℃。在这些条件下,使用280 nm紫外检测在5-500 μg/ml范围内获得了线性校准曲线。两种异构体的检测限均为0.1 μg/ml。该方法用于分析含头孢哌酮的不同药物制剂(剂量)和生物样品。