Szemán J, Csabai K, Kékesi K, Szente L, Varga G
CycloLab Cyclodextrin Research and Development Laboratory Ltd., P.O. Box 435, H-1525 Budapest, Hungary.
J Chromatogr A. 2006 May 26;1116(1-2):76-82. doi: 10.1016/j.chroma.2006.03.019. Epub 2006 Apr 3.
Novel stationary phases were prepared for separation of cyclodextrins and cyclodextrin derivatives by bonding substituted aromatic groups (phenyl and naphthyl) to the silica gel matrix. Both the electron-withdrawing (nitro) and the hydrogen-donor/acceptor (amide or carbamide) substituents of the phenyl group play essential role in the separation of cyclodextrins and cyclodextrin derivatives. On the basis of the comparison of experimental data obtained on different columns the N-(4-nitrophenyl)-carbamide group bonded silica gel stationary phase was selected as the most effective one for analysis of cyclodextrin derivatives. Improved separation potency was observed for hydroxypropylated, methylated and several other cyclodextrin derivatives compared with the previously and presently used stationary phases. Owing to the strong retention of cyclodextrins and its derivatives on the selected column, detection of their decomposition products was easily achieved. Determination of unsubstituted, natural cyclodextrin as an impurity in the cyclodextrin derivatives was implemented. Identification and characterization of cyclodextrin derivatives in industrial products could also be performed.
通过将取代的芳基(苯基和萘基)键合到硅胶基质上,制备了用于分离环糊精和环糊精衍生物的新型固定相。苯基的吸电子(硝基)和氢供体/受体(酰胺或脲)取代基在环糊精和环糊精衍生物的分离中都起着至关重要的作用。基于在不同柱上获得的实验数据的比较,选择了键合有N-(4-硝基苯基)-脲基团的硅胶固定相作为分析环糊精衍生物最有效的固定相。与先前和目前使用的固定相相比,观察到羟丙基化、甲基化和其他几种环糊精衍生物的分离效能有所提高。由于环糊精及其衍生物在所选柱上的强保留性,很容易实现其分解产物的检测。实现了对作为环糊精衍生物中杂质的未取代天然环糊精的测定。还可以对工业产品中的环糊精衍生物进行鉴定和表征。