Investigation of the novel mixed-mode stationary phase for capillary electrochromatography. I. Preparation and characterization of sulfonated naphthalimido-modified silyl silica gel.
Investigation of the novel mixed-mode stationary phase for capillary electrochromatography. I. Preparation and characterization of sulfonated naphthalimido-modified silyl silica gel.
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用于毛细管电色谱的新型混合模式固定相的研究。
DOI：
10.1016/j.chroma.2004.05.008
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发表时间：
2004
期刊：
影响因子：
--
通讯作者：
N. Kuroda
中科院分区：
文献类型：
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作者：
K. Ohyama;Yumi Shirasawa;M. Wada;N. Kishikawa;Y. Ohba;K. Nakashima;N. Kuroda
制备了一种新型的3-（4-磺基-1，8-萘酰亚胺基）丙基改性硅胶（SNAIP）作为毛细管电色谱（CEC）固定相。SNAIP固定相上的磺酸基团有助于在低pH值下产生电渗流，并充当强阳离子交换剂。在CEC与SNAIP，混合模式的分离被预测，包括疏水和静电相互作用以及电泳迁移过程。为了解SNAIP的保留机理，系统研究了缓冲液pH、浓度和移动的组成对巴比妥类和苯二氮卓类药物的流动性和保留因子的影响。此外，还研究了巴比妥类药物在SNAIP上的保留行为，并与十八烷基硅胶（ODS）、苯基键合硅胶和3-（1，8-萘酰亚胺基）丙基改性硅胶上的保留行为进行了比较，以证实其保留机理中存在π-π相互作用。柱效大于85，000 N/m，硫脲、巴比妥酸盐、巴比妥酸盐等5种化合物保留时间的相对标准偏差小于2.5%（n = 4）。在20 kV电压下，以5 mM磷酸盐（pH3.8）和40%甲醇为移动的流动相，5种巴比妥类药物在3 min内达到基线分离。
A novel packing material, 3-(4-sulfo-1,8-naphthalimido)propyl-modified silyl silica gel (SNAIP), was prepared for the use as a stationary phase of capillary electrochromatography (CEC). The sulfonic acid groups on SNAIP stationary phase contributed to the generation of electroosmotic flow (EOF) at low pH and served as a strong cation-exchanger. In CEC with SNAIP, a mixed-mode separation was predicted, comprising hydrophobic and electrostatic interactions as well as electrophoretic migration process. In order to understand the retention mechanism on SNAIP, effects of buffer pH, concentration, and mobile phase composition on EOF mobility and the retention factors of barbiturates and benzodiazepines were systematically investigated. Moreover, the retention behavior of barbiturates on SNAIP was investigated and compared with those on octadecyl silica (ODS), phenyl-bonded silica, and 3-(1,8-naphthalimido)propyl-modified silyl silica gel to confirm the presence of π–π interaction on its retention mechanism. It was observed that a column efficiency was more than 85,000N/m for retained compounds and the relative standard deviations for the retention times of EOF marker, thiourea, and five barbiturates were below 2.5% (n = 4). Under an applied voltage of 20kV and a mobile phase consisted of 5mM phosphate (pH 3.8) and 40% methanol, the baseline separation of five barbiturates was achieved within 3min.
在装有触手弱阳离子交换剂颗粒的柱上对肽进行毛细管电色谱分析。
DOI：
10.1016/s0021-9673(02)00070-5
发表时间：
2002
期刊：
Journal of chromatography. A
影响因子：
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作者：
Zhang,Jian;Zhang,Shuhong;Horváth,Csaba
通讯作者：
Horváth,Csaba