Journal of Chromatography A, 1035 (2004) 237–247 Evaluation of fast gas chromatography and gas chromatography–mass spectrometry in the analysis of lipids Luigi Mondello a,∗ , Alessandro Casilli a , Peter Quinto Tranchida a , Rosaria Costa b , Biagina Chiofalo b , Paola Dugo c , Giovanni Dugo a a Dipartimento Farmaco-Chimico, Facoltà di Farmacia, Università di Messina, Viale Annunziata, 98168 Messina, Italy b Dip. Mo.Bi.Fi.P.A.—Sez. Zootecnica, Polo Universitario dell’ Annunziata, Università di Messina, Viale Annunziata, 98168 Messina, Italy c Dipartimento di Chimica Organica e Biologica, Facoltà di Scienze MM.FF.NN., Università di Messina, Salita Sperone, 98165 Messina, Italy Received 6 October 2003; received in revised form 16 February 2004; accepted 19 February 2004 Abstract Fast and conventional gas chromatography (GC) techniques were applied to nine different lipidic matrices (butter, lard, tallow, and peanut, corn, sunflower, soya, olive, menhaden oils). Simultaneous methylic transesterification was performed on all samples prior to GC analysis. Several practical aspects concerning high speed analysis were investigated, such as the great increase in linear velocity, the use of fast temperature ramps, column sample capacity and detection systems. Analytical results showed certain losses in resolution, balanced by a consistent reduction in analysis time. The actual time savings were variable (60–70 min) as they were dependent on the complexity of the sample while the speed enhancement factor was equal to 10.5. Peak identification was achieved by means of different information sources, such as fast GC–mass spectrometry (MS), linear retention indices and comprehensive two-dimensional (2D) gas chromatography group patterns. The method developed was shown to be applicable in routine applications on complex natural samples. © 2004 Elsevier B.V. All rights reserved. Keywords: Gas chromatography, fast; Gas chromatography, comprehensive two-dimensional; Lipids; Fatty acid methyl esters 1. Introduction Lipids are used on a daily basis in our diet, consumed either as foods constituents or as condiments, and they have a fundamental importance in keeping us in good health. From a physiological standpoint, they play a role in several biochemical functions, such as constituents of biological membranes, vitamins, hormones, bile acids and as energy suppliers. In the last several years, the correlation between lipidic intake and health has been highlighted by several works regarding the links between cardiovascular diseases and a diet rich in saturated fatty acids (SFAs) [1–3]. This has led some nutritionists to emphasize the potential benefits of the Mediterranean diet, rich in vegetables, sea products and ex- travirgin olive oil. All these food products, in fact, contain a consistent amount of monounsaturated fatty acids (MUFAs) ∗ Corresponding author. Tel.: +390-090-676-6536; fax: +390-090-676-6532. E-mail address: lmondello@pharma.unime.it (L. Mondello). and essential fatty acids (EFAs), the so-called “good lipids”, due to their capability of hindering the formation of athero- matose plaques. On the other hand, the assumption of a diet rich in polyunsaturated fatty acids (PUFAs) and SFAs is not recommended, as the former tend to oxidize while the latter to settle in blood vessel walls. For the aforementioned rea- sons, there is a need to increase the knowledge about lipids in food, and analytical chemistry can be a precious support to both medicine and food science. The determination of the fatty acid composition in fats and oils, present mainly as triacylglycerols, is generally achieved by open tubular column (OTC) gas chromatogra- phy via methylic transesterification of the lipidic matrix [4]. This well-established conventional GC method produces ef- fective results but has one substantial limitation: the cost in time. In fact, satisfactory separations concerning moderately complex matrices such as lipids, can take an hour or more. This factor becomes particularly important for those labo- ratories where a great number of analyses are carried out and/or where there is a need for quick results. The growing necessity, over the years, for fast GC techniques has seen the 0021-9673/$ – see front matter © 2004 Elsevier B.V. All rights reserved. doi:10.1016/j.chroma.2004.02.058