Dipartimento Farmaco-Chimico, Facoltà di Farmacia, Università di Messina, Viale Annunziata, 98168-Messina, Italy.
Anal Chem. 2011 Oct 15;83(20):7947-54. doi: 10.1021/ac202012u. Epub 2011 Sep 27.
The present research is focused on the evaluation, in terms of efficiency and polarity, of a recently introduced gas chromatography (GC) column, coated with a 1,12-di(tripropylphosphonium) dodecane bis(trifluoromethansulfonyl) amide ionic-liquid stationary phase (SLB-IL59) and its application to the analysis of a complex essential oil. The ionic liquid column demonstrated very good efficiency, in terms of plate number, and a polarity close to that of the 100% poly(ethyleneglycol) stationary phase. In this preliminary evaluation, the SLB-IL59 30 m column was subjected to bleeding measurements, by means of conventional gas chromatography/mass spectrometry (GC/MS) and, in addition, of comprehensive 2D GC. The SLB-IL59 column (30 m × 0.20 μm d(f), 0.25 mm i.d.) was then evaluated in the analysis of typical essential oil constituents, in the form of pure standard compounds. Resolution toward several analytes was measured and the results were compared to those obtained with both apolar [silphenylene polymer, equivalent to poly(5% diphenyl/95% dimethylsiloxane)] and medium-polarity [100% poly(ethyleneglycol)] stationary phases, namely, the most common columns employed in the analysis of essential oils; peak symmetry, for different essential oil constituents, was also measured and expressed through tailing factors (at 10% of peak height). The final part of the investigation was devoted to the GC/MS analysis of lemon essential oil, with GC-flame ionization detection (FID) used for quantification. Linear retention indices of all the identified compounds were determined, and the data obtained were compared to those attained on the apolar and "wax" columns. The results obtained in the present investigation reveal the great potential of this novel stationary phase, as a medium-polarity alternative, in the analysis of essential oils.
本研究旨在评估一种新引入的气相色谱(GC)柱,该柱涂有 1,12-二(三丙基膦)十二烷双(三氟甲烷磺酰基)酰胺离子液体固定相(SLB-IL59),从效率和极性两个方面进行评价,并将其应用于复杂精油的分析。离子液体柱在板数方面表现出非常好的效率,极性接近于 100%聚乙二醇固定相。在这个初步评估中,通过常规气相色谱/质谱(GC/MS)和二维气相色谱(2D GC)对 SLB-IL59 30 m 柱进行了渗滤测量。然后,将 SLB-IL59 柱(30 m×0.20 μm d(f),0.25 mm i.d.)用于分析典型的精油成分,以纯标准化合物的形式进行。测量了对几种分析物的分辨率,并将结果与非极性[硅菲聚合物,相当于聚(5%二苯基/95%二甲基硅氧烷)]和中极性[100%聚乙二醇]固定相(即最常用于分析精油的常用柱)的结果进行了比较;还测量了不同精油成分的峰对称性,并通过拖尾因子(在峰高的 10%处)表示。研究的最后一部分致力于柠檬精油的 GC/MS 分析,使用 GC-火焰离子化检测(FID)进行定量。确定了所有鉴定化合物的线性保留指数,并将获得的数据与非极性和“蜡”柱获得的数据进行了比较。本研究的结果表明,这种新型固定相作为一种中极性替代品,在精油分析中具有巨大的潜力。