Mondello Luigi, Tranchida Peter Quinto, Dugo Paola, Dugo Giovanni
Dipartimento Farmaco-Chimico, Facoltà di Farmacia, Università di Messina, viale Annunziata, 98168 Messina, Italy.
J Pharm Biomed Anal. 2006 Aug 28;41(5):1566-70. doi: 10.1016/j.jpba.2006.01.027. Epub 2006 Feb 24.
The present research is focussed on the optimization of a fast and economically convenient method for the sample preparation and gas chromatographic separation of fatty acids contained in lipidic samples. This, as part of a wider project that has, as ultimate goal, the automation of this specific analytical procedure. The developed approach was applied to the analysis of cod liver oil, a highly complex lipid characterized by a wide nutritional interest. Derivatization was carried out by using low quantities (microL amounts) of a reagent and solvent, while the derived fatty acid methyl esters (FAMEs) were separated in 120 s on a 10 m x 0.1 mm i.d. polar micro-bore column. The total analysis time required for six samples was approximately 45 min (7.5 min/sample), considering a simultaneous process of methylation and GC separation of previously prepared samples. The results obtained were compared to those derived from conventional applications on the same sample. With regard to the validation of the rapid method, peak area/retention time repeatability, linear range, limit of detection (LOD) and quantitation (LOQ) were determined. Peak assignment was carried out by exploiting bidimensional group-type mapping information obtained in a comprehensive gas chromatographic application.
本研究聚焦于优化一种快速且经济便捷的方法,用于脂质样品中脂肪酸的样品制备及气相色谱分离。这是一个更广泛项目的一部分,该项目的最终目标是实现这一特定分析程序的自动化。所开发的方法应用于鱼肝油分析,鱼肝油是一种具有广泛营养价值的高度复杂脂质。衍生化过程使用少量(微升量)试剂和溶剂,而衍生的脂肪酸甲酯(FAMEs)在一根10 m×0.1 mm内径的极性微径柱上于120秒内分离。考虑到对先前制备样品进行甲基化和气相色谱分离的同步过程,六个样品所需的总分析时间约为45分钟(每个样品7.5分钟)。将所得结果与同一样品常规分析方法的结果进行比较。关于该快速方法的验证,测定了峰面积/保留时间重复性、线性范围、检测限(LOD)和定量限(LOQ)。通过利用在全二维气相色谱应用中获得的二维基团类型映射信息进行峰归属。