Automated sample preparation and fast GC–MS determination of fatty acids in blood samples and dietary supplements

• Published in: Analytical and bioanalytical chemistry 2022-12, Vol.414 (29-30), p.8423-8435
• Main Authors: Ferracane, Antonio, Aloisi, Ivan, Galletta, Micaela, Zoccali, Mariosimone, Tranchida, Peter Q., Micalizzi, Giuseppe, Mondello, Luigi
• Format: Article
• Language: English
• Subjects: Analysis; Analytical Chemistry; Biochemistry; Blood; Blood plasma; Characterization and Evaluation of Materials; Chemistry; Chemistry and Materials Science; Composition; Dietary supplements; Esters; Fatty acid methyl esters; Fatty acids; Fish oils; Food Science; Gas chromatography; Ions; Laboratory Medicine; Mass spectrometry; Mass spectroscopy; Monitoring/Environmental Analysis; Optimization; Polyethylene glycol; Qualitative analysis; Regression coefficients; Research Paper; Sample preparation; Stationary phase
• ISSN: 1618-2642; 1618-2650
• DOI: 10.1007/s00216-022-04379-8

The present research is focused on the optimization of an automatized sample preparation and fast gas chromatography–mass spectrometry (GC-MS) method for the analysis of fatty acid methyl esters (FAMEs) in blood samples and dietary supplements, with the primary objective being a significant reduction of the analysis time and, hence, an enhanced sample throughput. The mass spectrometer was operated in the scan/selected ion monitoring (SIM) acquisition method, thus enabling the obtainment of qualitative and (highly sensitive) quantitative data. The separation of FAMEs was obtained in about 11 min by using a micro-bore column of dimensions 15 m × 0.10 mm ID × 0.10 µm d f with a polyethylene glycol stationary phase. The novelty of the research involves reducing analysis time by using the novel fast GC–MS method with increased identification reliability and sensitivity in a single chromatographic run. With regard to the figures of merit, linearity, accuracy, and limits of detection (LoD) and quantification (LoQ) were determined. Specifically, regression coefficients were between 0.9901 and 0.9996; the LoDs ranged from 0.05 to 1.02 µg g −1 for the blood analysis method, and from 0.05 to 0.26 mg g −1 in the case of the dietary supplement approach. With respect to LoQs, the values were in the ranges of 0.15–3.39 µg g −1 and 0.15–0.86 mg g −1 for blood and dietary supplements analysis methods, respectively. Accuracy was evaluated by analyzing certified reference materials (human plasma, fish oil). Graphical abstract