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

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 reductio...

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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
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description 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
doi_str_mv 10.1007/s00216-022-04379-8
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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
title Automated sample preparation and fast GC–MS determination of fatty acids in blood samples and dietary supplements
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