Castro-Puyana María, Crego Antonio L, Marina M Luisa
Departamento de Química Analítica, Facultad de Química, Universidad de Alcalá, Alcalá de Henares, Madrid, Spain.
Electrophoresis. 2006 Feb;27(4):887-95. doi: 10.1002/elps.200500347.
The four stereoisomers of itraconazole were resolved for the first time by EKC using a CD as chiral selector. A study on the enantiomeric separation ability of different neutral CDs was carried out. Heptakis-2,3,6-tri-O-methyl-beta-CD was shown to provide the highest values for the enantiomeric resolution. The influence of some experimental conditions, such as pH, chiral selector concentration, and temperature, on the enantiomeric separation was also studied. The use of a 100 mM phosphate buffer (pH 2.5), 30 mM in heptakis-2,3,6-tri-O-methyl-beta-CD together with an applied voltage of 30 kV and a temperature of 20 degrees C enabled the separation of the enantiomers of itraconazole with high resolutions (Rs > 3.0). Finally, the method was validated and successfully applied to the quantitation of itraconazole in three pharmaceutical formulations.
首次采用环糊精作为手性选择剂，通过毛细管电泳拆分了伊曲康唑的四种立体异构体。开展了不同中性环糊精对映体拆分能力的研究。结果表明，七（2,3,6-三-O-甲基）-β-环糊精的对映体拆分度最高。还研究了一些实验条件，如pH值、手性选择剂浓度和温度，对映体拆分的影响。使用100 mM磷酸盐缓冲液（pH 2.5）、30 mM七（2,3,6-三-O-甲基）-β-环糊精，外加电压30 kV，温度20℃，能够实现伊曲康唑对映体的高分辨率拆分（Rs>3.0）。最后，该方法经过验证，并成功应用于三种药物制剂中伊曲康唑的定量分析。
