del Nozal M J, Toribio L, Bernal J L, Castaño N
Department of Analytical Chemistry, Faculty of Sciences, University of Valladolid, Prado de la Magdalena s/n, E-47005 Valladolid, Spain.
J Chromatogr A. 2003 Jan 31;986(1):135-41. doi: 10.1016/s0021-9673(02)01920-9.
The enantiomeric separation of triadimenol and triadimefon on a Chiralpak AD column using supercritical fluid chromatography, was studied in this work. The effect of different modifiers (methanol, ethanol and 2-propanol) was tested, with methanol and ethanol providing the best results for the enantiomeric separation of the two compounds. The enantioseparation of a mixture of triadimenol and triadimefon (six stereoisomers) was achieved in only 15 min using a gradient of ethanol, 200 bar, 35 degrees C and a flow-rate of 2 ml/min. The separation of triadimenol diastereoisomers on different achiral columns (diol, silica and ODS) was also investigated. In this case, the type of organic modifier to be used depended on the stationary phase, the Spherex Diol being the column that gave the best separation. Using this column, resolutions higher than 3 were obtained in analysis times of 5 min with any of the modifiers checked.
本研究采用超临界流体色谱法，在手性pak AD柱上对三唑醇和三唑酮进行对映体分离。测试了不同改性剂（甲醇、乙醇和异丙醇）的效果，甲醇和乙醇对这两种化合物的对映体分离效果最佳。使用乙醇梯度、200 bar、35℃和2 ml/min的流速，仅需15分钟就能实现三唑醇和三唑酮混合物（六种立体异构体）的对映体分离。还研究了三唑醇非对映异构体在不同非手性柱（二醇柱、硅胶柱和ODS柱）上的分离情况。在这种情况下，所用有机改性剂的类型取决于固定相，Spherex二醇柱是分离效果最佳的柱。使用该柱，在5分钟的分析时间内，用任何一种检测过的改性剂都能获得高于3的分离度。
