Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, University of Messina, Messina, Italy.
Chemistry Institute, UFRGS, Porto Alegre, RS, Brazil.
Anal Chim Acta. 2020 Apr 8;1105:231-236. doi: 10.1016/j.aca.2020.01.040. Epub 2020 Jan 21.
This preliminary research is focused on the task of defining an equivalent standard column set between cryogenic and flow-modulation comprehensive two-dimensional gas chromatography (GC × GC) combined with mass spectrometry (MS). Cryogenic modulation (CM) was carried out by using a loop-type device, while the flow modulator used was a seven-port wafer chip, equipped with an external accumulation loop. Initially, a common low-polarity + mid-polarity CM GC × GC column set was selected (30 m × 0.25 mm ID × 0.25 μm d + 1.5 m × 0.25 mm ID × 0.25 μm d), a method was developed, and a GC × GC-MS fingerprint was attained (on a sample of bio-oil derived from coconut fibers). After, a column set with the same stationary phases was selected for the flow modulation GC × GC-MS method (20 m × 0.18 mm ID × 0.18 μm d + 5 m × 0.32 mm ID × 0.25 μm d), with the capability to provide a-similar-as-possible separation. A side-by-side measurement of several chromatography parameters (efficiency, peak capacity, resolution, peak widths, retention factors, elution temperatures) was made.
本初步研究集中于定义低温与流动调制全二维气相色谱(GC×GC)与质谱联用(MS)之间等效标准柱集的任务。低温调制(CM)通过使用环型装置进行,而使用的流调制器是七端口晶圆芯片,配备外部积集环。最初,选择了常用的低极性+中极性 CM GC×GC 柱集(30m×0.25mm ID×0.25μm d+1.5m×0.25mm ID×0.25μm d),开发了一种方法,并获得了 GC×GC-MS 指纹图谱(在椰子纤维衍生的生物油样品上)。之后,为流动调制 GC×GC-MS 方法选择了具有相同固定相的柱集(20m×0.18mm ID×0.18μm d+5m×0.32mm ID×0.25μm d),其具有提供尽可能相似分离的能力。对几个色谱参数(效率、峰容量、分辨率、峰宽、保留因子、洗脱温度)进行了并排测量。