CAJ | 학술논문

制备了1 μm无孔硅胶颗粒.通过电动填充法得到总长度为45 cm(固定相填充长度为20 cm)、内径为100 μm的毛细管色谱柱.以乙腈-水体系作为流动相,详细考察了碱性化合物在该色谱柱上的加压电色谱(pCEC)分离性能,讨论了流动相比例、缓冲液浓度、pH值及操作电压等因素对分离的影响.实验结果表明,裸硅胶柱在乙腈-水体系分离碱性样品中表现出典型的反相色谱分离性能;缓冲液浓度的改变则对分离影响不大.当pH值改变时,碱性化合物的解离程度发生变化,它们与固定相之间的作用力发生变化,使得分离度发生相应的变化.分离柱效随施加电压的增加而增加,在 1 kV 电压下,裸硅胶柱对邻甲苯胺的柱效为 35 000理论塔板/m.
제비료1 μm무공규효과립.통과전동전충법득도총장도위45 cm(고정상전충장도위20 cm)、내경위100 μm적모세관색보주.이을정-수체계작위류동상,상세고찰료감성화합물재해색보주상적가압전색보(pCEC)분리성능,토론료류동상비례、완충액농도、pH치급조작전압등인소대분리적영향.실험결과표명,라규효주재을정-수체계분리감성양품중표현출전형적반상색보분리성능;완충액농도적개변칙대분리영향불대.당pH치개변시,감성화합물적해리정도발생변화,타문여고정상지간적작용력발생변화,사득분리도발생상응적변화.분리주효수시가전압적증가이증가,재 1 kV 전압하,라규효주대린갑분알적주효위 35 000이론탑판/m.
Bare nonporous silica particles with diameter around 1 μm were prepared.A 20 cm section of a total length of 45 cm capillary (100 μm i.d.) was packed electrokinetically and the separation performance of basic compounds was investigated in the pressurized capillary electrochromatography (pCEC) system using 1 μm nonporous bare silica spheres as stationary phase and acetonitrile-water as mobile phase.The effects of the composition of the mobile phase,the concentration of the buffer,pH value,applied voltage and so on on the separation performance were investigated.The experimental results demonstrated that the bare silica column showed a typical reversed phase separation mechanism when it was used for separation of basic compounds.The separation performance changed slightly with changing buffer concentration.Since the degree of dissociation of the basic compounds depended greatly on the pH value,the interaction between the compounds and stationary phase changed with the changing of pH value,thereby changing the resolution of the compounds.The separation performance increased with the increase of applied voltage.A column efficiency of 35 000 for o-toluidine was obtained when a voltage of 1 kV was applied.