Jandera P, Komers D, Guiochon G
Department of Analytical Chemistry, University of Pardubice, Czech Republic.
J Chromatogr A. 1998 Feb 13;796(1):115-27. doi: 10.1016/s0021-9673(97)01102-3.
To investigate the effects of various parameters on the production rate and on the recovery yield in overloaded reversed-phase gradient-elution chromatography, band profiles of binary mixtures of phenol and o-cresol were calculated using the experimental parameters of the distribution isotherms determined by binary frontal analysis. The effects of the feed volume and of the steepness of a continuous gradient (gradient time) of methanol in aqueous-organic mobile phases on the separation were studied. If the sample feed in a solvent with weak elution strength is used, combined effects of on-column enrichment, frontal chromatography and sharpening of the later eluted bands may enhance the production rate and the recovery yield. Steep continuous gradients offer better results than isocratic elution if the feed is dissolved in water and injected into the mobile phase with a higher elution strength, because larger volumes of dilute feed can be separated with high recovery yields.
为了研究过载反相梯度洗脱色谱中各种参数对产率和回收率的影响，使用二元迎头分析测定的分配等温线实验参数，计算了苯酚和邻甲酚二元混合物的谱带轮廓。研究了进样体积和水 - 有机流动相中甲醇连续梯度（梯度时间）的陡度对分离的影响。如果使用在具有弱洗脱强度的溶剂中进样的样品，柱上富集、迎头色谱和后洗脱谱带锐化的综合作用可能会提高产率和回收率。如果将进样溶解在水中并注入具有较高洗脱强度的流动相中，陡峭的连续梯度比等度洗脱能提供更好的结果，因为更大体积的稀进样可以以高回收率进行分离。
