Laboratorio de Investigación y Desarrollo de Métodos Analíticos, LIDMA, Facultad de Ciencias Exactas, Universidad Nacional de La Plata, 47 and 115 (B1900AJL), La Plata, Argentina.
Laboratorio de Investigación y Desarrollo de Métodos Analíticos, LIDMA, Facultad de Ciencias Exactas, Universidad Nacional de La Plata, 47 and 115 (B1900AJL), La Plata, Argentina; División Química Analítica, F. Ciencias Exactas, UNLP, 47 and 115 (B1900AJL), La Plata, Argentina.
J Chromatogr A. 2022 Jun 21;1673:463126. doi: 10.1016/j.chroma.2022.463126. Epub 2022 May 10.
This work demonstrates the potential of two-dimensional liquid chromatography (2D-LC) to increase the resolution capacity of multiple pesticides in a single analysis of samples that contain both chiral and achiral compounds. The setup is based on the combination of a chiral column in the first dimension and an achiral column in the second dimension using the on-line full comprehensive mode (LC × LC). This method was optimized for the separation of 24 pesticides (17 chiral and 7 achiral). The 2D-LC system was built with an active flow splitter pump in order to easily adjust the volume of sample transferred to the second dimension and to select and optimize independently the flow rate in the first dimension. The first-dimension optimization involved the comparison of enantioresolution abilities of three different polysaccharides chiral stationary phases as well as different elution conditions, while in the second-dimension parameters like stationary phase and organic modifier were explored. Other experimental variables that influence the two-dimensional peak capacity (orthogonality, sampling frequency, shift gradients, etc.) are discussed.
本工作展示了二维液相色谱（2D-LC）在单一分析中增加手性和非手性化合物样品中多种农药分辨率能力的潜力。该设置基于在第一维中使用手性柱和在第二维中使用非手性柱的在线全综合模式（LC×LC）组合。该方法针对 24 种农药（17 种手性和 7 种非手性）的分离进行了优化。2D-LC 系统采用主动流量分配器泵，以便于调整转移到第二维的样品体积，并独立选择和优化第一维的流速。第一维的优化涉及比较三种不同多糖手性固定相的手性拆分能力以及不同的洗脱条件，而在第二维中则探索了固定相和有机溶剂等参数。还讨论了影响二维峰容量的其他实验变量（正交性、采样频率、梯度位移等）。
