Sciarrone Danilo, Tranchida Peter Quinto, Costa Rosaria, Donato Paola, Ragonese Carla, Dugo Paola, Dugo Giovanni, Mondello Luigi
Dipartimento Farmaco-chimico, Facoltà di Farmacia, Università di Messina, Messina, Italy.
J Sep Sci. 2008 Oct;31(19):3329-36. doi: 10.1002/jssc.200800293.
The present research is focused on the offline combination of normal-phase LC to double-oven GC x GC-quadrupole MS. Initially, a diesel sample was subjected to automated LC x GC in order to define the elution windows of four fractions, viz., saturated hydrocarbons, monocyclic aromatics, dicyclic aromatics, tri- + tetracyclic aromatics; each fraction was collected exploiting the LC system in a further analysis and subjected to large-volume-injection-GC x GC analysis using an apolar-polar column combination. The GC x GC operational conditions were tuned in relation to the specific separation requirements of each heart-cut. The main benefits of what can be defined as offline LC-GC x GC were: (i) the high first-dimension LC selectivity; (ii) the injection of high sample amounts in the GC x GC system, enabling the detection and quantification of a series of low-amount diesel constituents; (iii) improved GC x GC operational conditions for each heart-cut with respect to direct GC x GC.
本研究聚焦于正相液相色谱与双炉气相色谱-质谱联用仪的离线联用。首先，对柴油样品进行自动液相色谱-气相色谱分析，以确定四个馏分的洗脱窗口，即饱和烃、单环芳烃、二环芳烃、三环+四环芳烃；利用液相色谱系统收集每个馏分，以便进一步分析，并使用非极性-极性柱组合进行大体积进样-气相色谱-质谱分析。根据每个中心切割馏分的特定分离要求调整气相色谱-质谱联用仪的操作条件。可定义为离线液相色谱-气相色谱-质谱联用的主要优点有：（i）一维液相色谱的高选择性；（ii）在气相色谱-质谱联用系统中进样大量样品，能够检测和定量一系列低含量的柴油成分；（iii）相对于直接气相色谱-质谱联用，每个中心切割馏分的气相色谱-质谱联用操作条件得到改善。
