Divjak Blaz, Goessler Walter, Haddad Paul R, Novic Milko
LEK, Pharmaceuticals, Ljubljana, Slovenia.
J Chromatogr A. 2003 Aug 1;1008(1):89-96. doi: 10.1016/s0021-9673(03)00976-2.
Ion chromatographic analysis of ions in samples containing complex matrix composition strongly depends on the on-column co-processes caused by sample matrix components. In the present publication studies of different separation phenomena in cation-exchange chromatography are described. The studies were performed at 'non-linear' chromatographic conditions, when the concentration of matrix (interfering) ions significantly exceeded the concentration of the eluent ions. During the research work, the processes already identified in anion-exchange chromatography, i.e. self-elution, on-column change of the eluent and sample-induced micro-gradient elution were used to explain the chromatographic behavior of alkaline and earth-alkaline cations when samples with high matrix cation concentration were analyzed. When present at higher concentrations, the ammonium cation was found to cause self-elution (NH4+ fraction) as well as on-column eluent neutralization due to its ability to diffuse into/back from the porous core of the stationary phase (NH3 fraction). Co-elution of a matrix component and analytes of interest caused spectroscopic interferences that additionally influenced the peak shape of each individual analyte.
对含有复杂基质成分的样品中的离子进行离子色谱分析,在很大程度上取决于样品基质成分引起的柱上共过程。本出版物描述了阳离子交换色谱中不同分离现象的研究。这些研究是在“非线性”色谱条件下进行的,此时基质(干扰)离子的浓度显著超过洗脱液离子的浓度。在研究工作中,利用阴离子交换色谱中已确定的过程,即自洗脱、洗脱液的柱上变化和样品诱导的微梯度洗脱,来解释分析高基质阳离子浓度样品时碱金属和碱土金属阳离子的色谱行为。当铵阳离子浓度较高时,由于其能够扩散进入固定相的多孔核/从固定相的多孔核扩散出来(NH₃部分),发现它会导致自洗脱(NH₄⁺部分)以及柱上洗脱液中和。基质成分与目标分析物的共洗脱会引起光谱干扰,这进一步影响了每个单独分析物的峰形。