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 x 0.10 mm ID x 0.10 mu m 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 mu g 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 mu g 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).

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

Ferracane, Antonio
Primo
;
Aloisi, Ivan
Secondo
;
Galletta, Micaela;Zoccali, Mariosimone;Tranchida, Peter Q;Micalizzi, Giuseppe
Penultimo
;
Mondello, Luigi
Ultimo
2022-01-01

Abstract

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 x 0.10 mm ID x 0.10 mu m 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 mu g 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 mu g 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).
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11570/3248355
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