Zhao Yan, Yang Xingbin, Sun Xiaoli, Jiang Ru, Zhang Shengyong
Department of Chemistry, Fourth Military Medical University, Xi'an 710032, China.
J Chromatogr A. 2006 Mar 10;1108(2):258-62. doi: 10.1016/j.chroma.2006.01.022. Epub 2006 Feb 3.
A new capillary electrophoretic method was developed for enantiomeric separation and optical impurity analysis of three synthetic 2,3-dihydroxy-3-phenylpropionate compounds using native beta-cyclodextrin (beta-CD) as chiral selector and borate as a background electrolyte. The separation was carried out in uncoated capillary (58.5 cm x 75 microm I.D., effective length 48.5 cm). The results showed that beta-CD as the chiral selector exhibited good enantioselectivity and the baseline separation was obtained at pH 9.8, 200 mM borate buffer containing 1.7% beta-CD at applied voltage 15 kV and capillary temperature 20 degrees C within 15 min. The precision of each tested compound was less than 1.0% at migration time and 5.0% in corrected peak area and the accuracy of the method was in the range of 98.7-105%. Furthermore, the developed method was successfully applied to the determination of the undesirable trace (2S,3R)-(+)-form impurity in the synthetic (2R,3S)-(-)-2,3-dihydroxy-3-phenylpropionate samples.
建立了一种新的毛细管电泳方法，以天然β-环糊精（β-CD）作为手性选择剂，硼酸盐作为背景电解质，用于三种合成的2,3-二羟基-3-苯基丙酸酯化合物的对映体分离和光学杂质分析。分离在未涂层毛细管（58.5 cm×75μm内径，有效长度48.5 cm）中进行。结果表明，β-CD作为手性选择剂表现出良好的对映选择性，在pH 9.8、含有1.7%β-CD的200 mM硼酸盐缓冲液中，于15 kV的施加电压和20℃的毛细管温度下，15分钟内可实现基线分离。各被测化合物迁移时间的精密度小于1.0%，校正峰面积的精密度为5.0%，该方法的准确度在98.7%至105%范围内。此外，所建立的方法成功应用于合成的（2R,3S）-（-）-2,3-二羟基-3-苯基丙酸酯样品中痕量（2S,3R）-（+）-型杂质的测定。
