Fast Triacylglycerol Fingerprinting in Edible Oils by Subcritical Solvent Chromatography

Abstract

Supercritical fluid chromatography (SFC) has witnessed a resurge of interest in the last decade, motivated by substantial progress in hardware capabilities and the development of specifically tailored packing materials. Meanwhile, the technique has been transitioning to the use of mobile phases in which an organic co-solvent is mixed to carbon dioxide under subcritical conditions (subFC). The use of a mobile phase modifier will also affect the selectivity, and extend the range of SFC-amenable compounds, including lipids. In this research, a subFC method was developed for the separation of triacylglycerols (TAGs) in edible oils of vegetable origin, namely borage, corn, hazelnut, olive, palm, peanut, and soybean oil. For all the samples investigated, elution of the TAG species was achieved within 8 min, the only exception being borage oil (14 min run), characterized by TAGs spanning in a wide range of partition number (PN 36–56), as constituted by fatty acids differing for alkyl chain lengths (CN 14–24), and degree of unsaturation (DB 0–9). The coupling to mass spectrometry (MS) detection allowed for the average parameters of fatty acid composition to be derived in the oil TAG constituents. A total of 121 TAGs were identified by subFC-MS, with reduced analysis time and solvent consumption (1.5 mL per analysis) compared to common chromatographic approaches. Key features of the method developed hereby are low toxicity, costs, and environmental impact. Notably, the achieved separations were conducted at room temperature, which is beneficial in terms of column life.