Sokoliess Torsten, Schönherr Janet, Menyes Ulf, Roth Ulrich, Jira Thomas
Institute of Pharmacy, Pharmaceutical/Medicinal Chemistry, Ernst-Moritz-Arndt-University of Greifswald, Friedrich-Ludwig-Jahn-Strasse 17, Greifswald D-17487, Germany.
J Chromatogr A. 2003 Dec 22;1021(1-2):71-82. doi: 10.1016/j.chroma.2003.09.014.
New HPLC phases with supramolecular selectors on the basis of calixarenes and resorcinarenes were investigated for the first time by means of empirically based test mixtures. The tests, originally developed for common reversed phases, were chosen to evaluate fundamental chromatographic properties of the new materials. In the first part of these studies three descriptors (hydrophobic retention capacity--k'(hyd), hydrophobic selectivity--alpha(hyd), steric selectivity--alpha(ster)) were determined. Except of higher alpha(ster) values and alpha(hyd) values with some methods for the resorcinarene phase the phases with supramolecular selectors were classified as less hydrophobic possessing lower hydrophobic and steric selectivities compared to three RP-C18 phases and a p-tert-butyl phenyl ether phase. The results were confirmed by means of a separation of geometric isomers of thioxanthenes. In contrast, in spite of lower k'(hyd) and alpha(hyd) values calixarene phases were more selective than the Kromasil-C18 phase in the separation of gestagenic and androgenic steroids due to specific interactions with the steroids of similar lipophilicity.
首次采用基于经验的测试混合物，对基于杯芳烃和间苯二芳烃的具有超分子选择剂的新型高效液相色谱固定相进行了研究。这些最初为普通反相固定相开发的测试，被用于评估新材料的基本色谱性能。在这些研究的第一部分，测定了三个描述符（疏水保留容量——k'(hyd)、疏水选择性——α(hyd)、空间选择性——α(ster)）。除了间苯二芳烃固定相的某些方法具有较高的α(ster)值和α(hyd)值外，与三个RP-C18固定相和一个对叔丁基苯醚固定相相比，具有超分子选择剂的固定相被归类为疏水性较低，具有较低的疏水和空间选择性。通过噻吨类几何异构体的分离证实了该结果。相比之下,尽管杯芳烃固定相的k'(hyd)和α(hyd)值较低，但由于与具有相似亲脂性的甾体发生特异性相互作用，在孕甾类和雄甾类甾体的分离中，杯芳烃固定相比Kromasil-C18固定相具有更高的选择性。
