A high throughput method for fatty acid profiling using simultaneous microwave-assisted extraction and derivatization followed by reversed fill/flush flow modulation comprehensive multidimensional gas chromatography

Abstract

The fatty acid composition of a food product provides information regarding the origin of the product and its overall quality, such as its nutritional value. This work proposes a fast and accurate method for preparing fatty acid methyl esters from a wide variety of food products by using a single-step microwave-assisted extraction and derivatization coupled to reversed fill/flush flow modulation comprehensive two-dimensional gas chromatography (GC×GC) – flame ionization detector (FID) to tentatively identify and quantify the individual fatty acid. The robustness of the GC×GC – FID platform was successfully assessed, as well as the reliability of the entire proposed procedure, assuring repeatability largely below 10%. The enhanced separation obtained by the use of GC×GC allowed for the identification of 81 FAMEs in a single run of 30 min. The fatty acid methyl esters profiles obtained with the proposed microwave-assisted extraction and derivatization were comparable with reference methods from the literature and the American Oil Chemistry Society. This method also proved to be a significant step towards a greener procedure than the reference one when evaluated based on the PrepAGREE metrics that have been recently proposed.

Keywords

• Fatty acid methyl esters (FAMEs)
• Microwave-assisted extraction
• Microwave-assisted derivatization
• Comprehensive two-dimensional gas chromatography (GC×GC)
• Reversed fill/flush flow modulation