Boggia Raffaella, Borgogni Cristina, Hysenaj Vilma, Leardi Riccardo, Zunin Paola
Department of Pharmacy - Unit of Pharmaceutical and Food Chemistry and Technology - University of Genoa - Via Brigata Salerno, 13 I-16147 Genoa, Italy.
Customs Agency for Liguria - Via Rubattino, 6 I-16126 Genoa, Italy.
Talanta. 2014 Feb;119:60-7. doi: 10.1016/j.talanta.2013.10.055. Epub 2013 Oct 31.
A new analytical method for fatty acid alkyl esters (FAAEs) determination by GC-MS in virgin olive oils is proposed. No sample preparation is required and FAAEs are directly thermo-desorbed and cryo-focalised in the cooled injector of a GC-MS (EI) instrument. The analytical conditions were optimized by Design of Experiment (DoE) techniques (an exploratory Plackett-Burman design followed by a factorial design on three selected variables). After the improvement of method performances, several samples of extra virgin and low quality virgin olive oils were analyzed both by the new method and by the Official EU Method of analysis. The application of Principal Component Analysis to the obtained results confirmed that the ability of the proposed method to discriminate between extra virgin and lower quality olive oils is at least equal to that of the Official Method, but the new method is faster, simpler, requires a much lower amount of organic solvents and significantly enhances method repeatability.
提出了一种通过气相色谱 - 质谱联用(GC - MS)测定初榨橄榄油中脂肪酸烷基酯(FAAEs)的新分析方法。该方法无需样品前处理,FAAEs可直接在GC - MS(EI)仪器的冷却进样器中进行热脱附和冷聚焦。通过实验设计(DoE)技术(先进行探索性的Plackett - Burman设计,然后对三个选定变量进行析因设计)优化分析条件。在方法性能得到改进后,采用新方法和欧盟官方分析方法对多个特级初榨和低质量初榨橄榄油样品进行了分析。对所得结果应用主成分分析证实,所提出的方法区分特级初榨和低质量橄榄油的能力至少与官方方法相当,但新方法更快、更简单,所需有机溶剂用量少得多,且显著提高了方法的重复性。