Dipartimento Farmaco-chimico, Facoltà di Farmacia, Università di Messina, viale Annunziata, 98168 Messina, Italy.
J Chromatogr A. 2009 Dec 18;1216(51):8992-7. doi: 10.1016/j.chroma.2009.10.066. Epub 2009 Oct 30.
The present research is focused on the GC-FID determination of fatty acid methyl esters (FAMEs) in diesel blends, by means of an ionic liquid stationary phase, characterized by a dicationic 1,9-di(3-vinyl-imidazolium)nonane bis(trifluoromethyl)sulfonylimidate structure (SLB-IL100). The high polarity of the ionic liquid stationary phase allowed the separation of the FAMEs, from the less-retained hydrocarbons, thus avoiding the requirement of a hydrocarbon LC pre-separation. The results derived from the analyses of a soybean FAMEs B20 sample, carried out on an SLB-IL100 conventional column (30 m x 0.25 mm i.d. x 0.20 mm d(f)), were compared with those attained on a polyethylene glycol column, of equivalent dimensions. Conventional and fast GC methods, for the analysis of FAMEs in diesel blends, were developed on an SLB-IL100 30 m x 0.25 mm i.d. x 0.20 microm d(f) and on an SLB-IL100 12 m x 0.10 mm i.d. x 0.08 microm d(f) column, respectively. The optimized IL methods were subjected to validation: retention time and peak area intra-day precision (n=5) were good, with CV % values lower than 0.08% and 4.9%, respectively. With regards to the quantitation of FAMEs in biodiesel blends, a five points calibration curve was constructed, using C(17:0) as internal standard.
本研究专注于通过离子液体固定相，通过二阳离子 1,9-二(3-乙烯基-咪唑基)壬烷双(三氟甲基磺酰基)亚胺盐结构(SLB-IL100)，对柴油混合物中的脂肪酸甲酯(FAME)进行 GC-FID 测定。离子液体固定相的高极性允许 FAME 与保留性较低的烃类分离，从而避免了烃类 LC 预分离的要求。在 SLB-IL100 常规柱(30 m x 0.25 mm id x 0.20 mm d(f))上分析大豆 FAMEs B20 样品时得出的结果与在等效尺寸的聚乙二醇柱上得出的结果进行了比较。在 SLB-IL100 30 m x 0.25 mm id x 0.20 microm d(f)和 SLB-IL100 12 m x 0.10 mm id x 0.08 microm d(f)柱上分别开发了用于柴油混合物中 FAMEs 分析的常规和快速 GC 方法。对优化后的 IL 方法进行了验证：日内精密度（n=5）良好，保留时间和峰面积的 CV%值均低于 0.08%和 4.9%。关于生物柴油混合物中 FAME 的定量，使用 C(17:0)作为内标构建了五点校准曲线。
