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

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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 × 0.10 mm ID × 0.10 µm df 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).

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Acknowledgements

The authors thank Merck Life Science and Shimadzu Corporations for their continuous support. The research was conducted within the PRIN 2017 “Cutting-edge analytical chemistry methodologies and bio-tools to boost precision medicine in hormone-related diseases” supported by the Ministry University and Scientific Research, Prot. 2017Y2PAB8a. The scholarship of Ivan Aloisi was funded by the “Italian Ministry for the University and Research (MIUR)” within the National Operative Project “Dottorati Innovativi con caratterizzazione Industriale” (CCI 2014IT16M2OP005). This article is based upon work from the Sample Preparation Task Force and Network, supported by the Division of Analytical Chemistry of the European Chemical Society.

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Authors and Affiliations

  1. Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, University of Messina, 98168, Messina, Italy

    Antonio Ferracane, Ivan Aloisi, Micaela Galletta, Peter Q. Tranchida, Giuseppe Micalizzi & Luigi Mondello

  2. Department of Mathematical and Computer Science, Physical Sciences and Earth Sciences, University of Messina, 98168, Messina, Italy

    Mariosimone Zoccali

  3. Chromaleont S.R.L., c/o Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, University of Messina, 98168, Messina, Italy

    Luigi Mondello

  4. Unit of Food Science and Nutrition, Department of Medicine, University Campus Bio-Medico of Rome, 00128, Rome, Italy

    Luigi Mondello

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  1. Antonio Ferracane
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  2. Ivan Aloisi
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Correspondence to Giuseppe Micalizzi.

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All procedures followed were in accordance with the ethical standards of the responsible committee on human experimentation (institutional and national) and with the Helsinki declaration of 1975 (in its most recently amended version).

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Ferracane, A., Aloisi, I., Galletta, M. et al. Automated sample preparation and fast GC–MS determination of fatty acids in blood samples and dietary supplements. Anal Bioanal Chem 414, 8423–8435 (2022). https://doi.org/10.1007/s00216-022-04379-8

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  • DOI: https://doi.org/10.1007/s00216-022-04379-8

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