School of Chemical Technology, Shenyang University of Chemical Technology, Shenyang, 110142, P. R. China.
J Sep Sci. 2021 Sep;44(17):3295-3304. doi: 10.1002/jssc.202100298. Epub 2021 Jul 11.
An open tubular capillary electrochromatography column was prepared by immobilizing β-cyclodextrin on the inner wall of pretreated capillary via noncovalent adsorption of polydopamine. The resulting coating layer on the capillary was characterized by scanning electron microscopy and Fourier transform infrared spectroscopy. Electroosmotic flow was studied to evaluate the variation of the immobilized columns. The prepared columns showed good chiral separation performance toward five proton pump inhibitors including lansoprazole, pantoprazole, tenatoprazole, rabeprazole, and omeprazole. The influences of β-cyclodextrin concentration, coating time, buffer pH, buffer concentration, and applied voltage on separation were investigated. In the optimum conditions, the enantiomers of five analytes were fully resolved within 15 min with high resolutions of 4.57 to 8.13. The method was extensively validated in terms of accuracy, precision, and linearity and proved to be robust. The relative standard deviation values for migration times and peak areas of the analytes representing intraday and interday were less than 1.9 and 3.6%, respectively. Further, the polydopamine/β-cyclodextrin coated capillary column could be successively used over 100 runs without showing significant decrease in the separation efficiency.
通过聚多巴胺的非共价吸附将β-环糊精固定在预处理毛细管的内壁上，制备了开管毛细管电色谱柱。通过扫描电子显微镜和傅里叶变换红外光谱对毛细管上的涂层进行了表征。研究了电动流动以评估固定化柱的变化。所制备的柱对包括兰索拉唑、泮托拉唑、替那拉唑、雷贝拉唑和奥美拉唑在内的五种质子泵抑制剂表现出良好的手性分离性能。考察了β-环糊精浓度、涂层时间、缓冲液 pH 值、缓冲液浓度和外加电压对分离的影响。在最佳条件下，五种分析物的对映异构体在 15 分钟内完全分离，分辨率高达 4.57 至 8.13。该方法在准确性、精密度和线性方面进行了广泛验证，证明是稳健的。分析物的迁移时间和峰面积的相对标准偏差值（日内和日间）分别小于 1.9%和 3.6%。此外，聚多巴胺/β-环糊精涂层毛细管柱可以在 100 次以上的使用中连续使用，而不会显著降低分离效率。
