Dipartimento Farmaco-chimico, Facoltà di Farmacia, Università di Messina, Viale Annunziata, 98168 Messina, Italy.
J Chromatogr A. 2010 Jun 18;1217(25):4160-6. doi: 10.1016/j.chroma.2010.01.040. Epub 2010 Jan 20.
The objective of the present research is directed towards the optimized use of a 50microm ID secondary column, in a comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry (GCxGC-qMS) system. The analytical aim was achieved by exploiting a split-flow GCxGC approach, and a rapid-scanning qMS instrument. The stationary phase combination consisted of an apolar (silphenylene polymer) 30mx0.25mm ID column, linked by means of a Y-union, to an MS-connected 1mx0.05mm ID polar one [poly(ethyleneglycol)], and to a 0.20mx0.05mm ID uncoated capillary segment; the latter was connected to a manually operated split-valve. It will be herein demonstrated that the split-flow GCxGC approach, successfully employed in previous H(2)-based, flame ionization detection experiments, provides equally satisfactory results using mass spectrometric detection and helium as carrier gas. An optimized split-flow GCxGC-qMS method was developed and exploited for the analysis of a perfume sample. The results attained were compared with those observed using the same analytical column combination, but with no flow-splitting. It was found that it is not convenient to employ a 50microm ID secondary column in a conventional GCxGC-MS instrument. On the contrary, the use a 50microm ID secondary column, in a split-flow, twin-oven system, provided a good performance. A recently developed comprehensive chromatography software was used for data processing.
本研究的目的是针对 50μm ID 二次柱的优化使用，在全二维气相色谱-四极杆质谱联用（GCxGC-qMS）系统中。通过采用分流式 GCxGC 方法和快速扫描 qMS 仪器实现了分析目标。固定相组合由非极性（硅苯撑聚合物）30mx0.25mm ID 柱组成，通过 Y 型接头与 MS 连接的 1mx0.05mm ID 极性柱[聚乙二醇]和 0.20mx0.05mm ID 未涂层毛细管段相连；后者连接到手动操作的分流阀。将证明，在以前基于 H（2）的火焰离子化检测实验中成功采用的分流式 GCxGC 方法，使用质谱检测和氦气作为载气同样可以获得令人满意的结果。开发并利用优化的分流式 GCxGC-qMS 方法分析了一种香水样品。将获得的结果与使用相同分析柱组合但不分流的结果进行了比较。结果表明，在传统的 GCxGC-MS 仪器中使用 50μm ID 二次柱并不方便。相反，在分流、双炉系统中使用 50μm ID 二次柱可以提供良好的性能。最近开发的综合色谱软件用于数据处理。
