Electrochromatography in chemically modified etched fused-silica capillaries.
Electrochromatography in chemically modified etched fused-silica capillaries.
复制标题
化学改性蚀刻熔融石英毛细管中的电色谱。
DOI：
10.1016/0021-9673(95)01320-2
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发表时间：
1996
期刊：
影响因子：
--
通讯作者：
Matyska,MT
中科院分区：
文献类型：
--
作者：
Pesek,JJ;Matyska,MT
本文介绍了一种新的电色谱方法，即用氟化氢铵腐蚀50 μm毛细管，然后用三乙氧基硅烷对新表面进行硅化反应，生成氢化物中间体，然后在铂络合物催化剂存在下用1-十八烯进行硅氢化反应。然后将C18键合相与裸毛细管、蚀刻的裸毛细管和氢化物蚀刻的毛细管进行比较，以确定是否存在任何溶质键合相相互作用。与缓激肽作为测试溶质，峰效率是非常相似的所有毛细管没有C18，但变得明显更广泛的有机部分时，连接到蚀刻的毛细管壁。当将甲醇加入到移动的相中时，肽和蛋白质的供试混合物显示出某些组分的保留时间较短，这是典型的反相行为。当四环素类混合物在C18毛细管上分离时，有或没有甲醇作为移动的相的一部分，也得到相同的结果。两种蛋白质保留时间的重现性为± 1.5%。几种中性化合物的一些结果表明，κ′值很小，但可测量。
A new method of electrochromatography is described in which a 50-μm capillary is etched with ammonium hydrogen difluoride, followed by modification of the new surface via a silation reaction with triethoxysilane to produce a hydride intermediate, and then subsequently subjected to hydrosilation using 1-octadecene in the presence of a platinum complex catalyst. The C18bonded phase is then compared with bare capillaries, etched bare capillaries and the hydride etched capillary to determine if any solute-bonded phase interactions are present. With bradykinin as a test solute, peak efficiencies are quite similar for all capillaries without C18but become noticeably broader when the organic moiety is attached to the etched capillary wall. A test mixture of peptides and proteins displays shorter retention for some of the components when methanol is added to the mobile phase which is typical of reversed-phase behavior. The same result is also obtained when a mixture of tetracyclines is separated on the C18capillary with and without methanol as part of the mobile phase. The reproducibility of retention times for two proteins is ±1.5%. A few results for several neutral compounds indicate small but measurable κ′ values.