Dugo Paola, del Mar Ramírez Fernández Maria, Cotroneo Antonella, Dugo Giovanni, Mondello Luigi
Dipartimento di Chimica Organica e Biologica, Facolta di Science, Università di Messina, Salita Sperone 31, 98166 Messina, Italy.
J Chromatogr Sci. 2006 Oct;44(9):561-5. doi: 10.1093/chromsci/44.9.561.
The present investigation is based on the evaluation of the performance of a comprehensive two-dimensional liquid chromatography (LCxLC) system during method optimization. The LCxLC set-up, operated in normal phase (NP) mode (adsorption) in the first dimension (1D) and reversed-phase (RP) mode in the second dimension (2D), is equipped with a 1D microbore silica column and a 2D monolithic C(18) column with a 10-port two position valve as the interface. A photodiode array detector is used after the 2D separation. A possible cause of peak distorsion because of the immiscibility of the mobile phases employed in the two dimensions is resolved. The optimization of the analytical run time and flow rate for both dimensions and the initial gradient in the 2D is carried out with various standard compounds. The potential and versatility of this LCxLC approach is demonstrated through the separation of 11 standard components, most of them allergens. The latter, which are characterized by a scattered distribution on the 2D space plane, underwent separation on both a hydrophobicity and polarity basis.
本研究基于在方法优化过程中对综合二维液相色谱（LCxLC）系统性能的评估。该LCxLC装置在第一维（1D）以正相（NP）模式（吸附）运行，在第二维（2D）以反相（RP）模式运行，配备有1D微径硅胶柱和2D整体式C18柱，并以一个10端口二位阀作为接口。二维分离后使用光电二极管阵列检测器。解决了由于二维中使用的流动相不互溶导致峰变形的一个可能原因。使用各种标准化合物对二维的分析运行时间、流速以及二维中的初始梯度进行了优化。通过分离11种标准成分（其中大部分是过敏原）证明了这种LCxLC方法的潜力和通用性。后者在二维空间平面上呈分散分布，基于疏水性和极性进行了分离。
