毛细管电色谱行为的初步考察  

Preliminary Investigation of Characteristics of Capillary Electrochro m atography

作　　者：芮建中[1] 邹汉法[1] 施维[1] 张丽华[1] 朱军[1] 

机构地区：[1]中国科学院大连化学物理研究所国家色谱研究分析中心,大连116011

出　　处：《中国药科大学学报》1999年第4期264-268,共5页Journal of China Pharmaceutical University

基　　金：国家杰出青年基金

摘　　要：用高压匀浆填充和高温烧结固定相法制备反相和混合型电色谱柱，初步考察了改变不同条件，包括电压、电解质种类、电解质浓度、有机试剂比例、样品溶剂组成和进样条件等，对电流、电渗流和柱效等反相电色谱行为的影响。电解质为磷酸二氢钠的流动相，电流值较大，且随电压变化明显，电流与电压之间存在较好的线性关系。当电解质浓度上升电渗流略呈下降趋势，柱效增大。乙腈浓度增加，硫脲的保留时间缩短。随着进样量的增大，柱效逐渐下降；以去离子水或以乙腈水（９０∶１０ ，ｖｖ） 为溶剂的样品，其柱效较高，而以乙腈水（５０∶５０ ，ｖｖ） 为溶剂的样品，其柱效相对其它样品较低。另外，心血管药物普罗帕酮及其代谢物５羟基普罗帕酮和硫脲能在混合型电色谱柱上４ ｍｉｎ 内达到快速分离。Capillary electrochromatography ( C E C) couples very high efficiencies associated with capillaryelectrophoresis( C E) and with high performance liquid chromatography( H P L C) . In this paper ,some characteristics ofreversed phase C E C, such as running current,linear velocity of electroosmotic flow( E O F) and column efficiencieswere studied . The influence of running voltage , electrolyte type , electrolyte concentrations , acentonitrileconcentrations ,injection conditions and the composition ofsample solventon the property of R P C E Cwas investigated . The fused silica capillary column with 75 μm inner diameter was packed with 3 μm O D Sstationary phase to 20 cm byultrasonic slurry pumped . The total length of capillary column was 27 cm . On line U V detector was used . A goodlinear relationship between the running current and applied voltage was obtained . The currents in phosphatic mobilephase were biggerthan in Tris mobile phase . The E O Fmonitored by using thiourea as a marker will be decreased whenthe electrolyte concentration increases . The higher the acetonitrile concentration was ,the higher the E O F was . Thecolumn efficienciesincreased as the electrolyte concentrations increasing ,but decreased asthe sample plug increasing . The shape of profile and the column efficiencies in samples which solvents were comprised by 90 % acetonitrile and10 % deioned water were better than in samples which solvents were comprised by 50 % acetonitrile and 50 % deionedwater . It isless than 4 min to separate propafenone ,5 hydroxy propafenone and thiourea in mixed packed C E Ccolumnusing a mobile phase with 5 m mol L Tris and 80 % acetonitrile∶deioned water(vv) . The highest efficiencies obtainedwas 140 000 plate per meter for a retained solute ,5 hydroxy propafenone .

关 键 词：毛细管电色谱 电渗流 柱效 硫脲 普罗帕酮 

分 类 号：R972[医药卫生—药品]