Pesek J J, Matyska M T, Cho S
Department of Chemistry, San Jose State University, CA 95192, USA.
J Chromatogr A. 1999 Jun 11;845(1-2):237-46. doi: 10.1016/s0021-9673(99)00154-5.
Fused silica capillaries with an I.D. of 20 microns are etched and then chemically modified by the silanization/hydrosilation method to attach an octadecyl moiety for use in electrokinetic chromatography. The etched capillaries after chemical modification are shown to have an anodic electroosmotic flow below pH 4.5. In comparison to bare 20 microns capillaries and unetched but chemically modified 20 microns capillaries, the etched C18 fused silica tubes show better separation of mixtures of lysozymes and cytochrome c's under identical conditions of buffer, pH and applied voltage. It was also demonstrated that this open tubular approach to capillary electrochromatography was amenable to a number of different types of basic compounds ranging in size from typical small amines to biomolecules. As expected, pH is an important variable that must be controlled in order to obtain an optimized separation. Reproducibility studies verify the stability of the silicon-carbon linkage produced in this modification method so that column lifetimes of at least 300 injections can be expected.
内径为20微米的熔融石英毛细管经过蚀刻，然后通过硅烷化/硅氢化方法进行化学修饰，以连接十八烷基部分，用于电动色谱分析。经化学修饰后的蚀刻毛细管在pH值低于4.5时呈现出阳极电渗流。与未蚀刻的20微米裸毛细管以及未蚀刻但经过化学修饰的20微米毛细管相比，蚀刻后的C18熔融石英管在相同的缓冲液、pH值和施加电压条件下，对溶菌酶和细胞色素c混合物的分离效果更好。还证明了这种用于毛细管电色谱的开管方法适用于多种不同类型的碱性化合物，其大小范围从典型的小胺到生物分子。正如预期的那样，pH值是一个重要变量，为了获得优化的分离效果必须加以控制。重现性研究证实了这种修饰方法中产生的硅-碳键的稳定性，因此预计柱寿命至少为300次进样。
