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Authentication of fish oil (omega-3) supplements using class-oriented chemometrics and comprehensive two-dimensional gas chromatography coupled to mass spectrometry

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Abstract

Food supplement authentication is an important concern worldwide due to the ascending consumption related to health benefits and its lack of effective regulation in underdeveloped countries, making it a target of fraudulent activities. In this context, this study evaluated fish oil supplements by comprehensive two-dimensional gas chromatography coupled to mass spectrometry (GC×GC–MS) to obtain fingerprints, which were used to build predictive models for automated authentication of the most popular products sold in Brazil. The authentication process relied on a one-class classifier model using data-driven soft independent modeling of class analogy (DD-SIMCA). The output of the model was a binary classifier: certified IFOS fish oils and non-certified ones — regardless of the source of adulteration. The compositional analysis showed a significant variation in the samples, which validated the need for reliable statistical models. The DD-SIMCA algorithm is still incipient in GC×GC studies, but it proved to be an excellent tool for authenticity purposes, achieving a chemometric model with a sensitivity of 100%, specificity of 98.6%, and accuracy of 99.0% for fish oil authentication. Finally, orthogonalized partial least square discriminant analysis (OPLS-DA) was used to identify the features that distinguished the groups, which ascertained the results of the DD-SIMCA model that IFOS-certified oils are positively correlated to omega-3 fatty acids, including eicosapentaenoic acid (EPA, C20:5 n-3) and docosahexaenoic acid (DHA, C22:6 n-3).

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Funding

This study was financed by ANP/PETROBRAS (Grant 2019/00209–3 and 2019/00210–1, Brazil), the National Council for Scientific and Technological Development (CNPq) (Grant 316202/2021–5), the São Paulo Research Foundation (FAPESP) (Grant 14/50867–3 and 20/01064–6), and the Coordination for the Improvement of Higher Education Personnel (CAPES) — Finance Code 001.

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Authors and Affiliations

  1. Institute of Chemistry, University of Campinas, Campinas, Brazil

    Rássius Alexandre Medeiro Lima, Sofia Madruga Marcondes Ferraz, Victor Gustavo Kelis Cardoso, Carlos Alberto Teixeira & Leandro Wang Hantao

  2. National Institute of Science and Technology in Bioanalytics (INCTBio), Campinas, Brazil

    Rássius Alexandre Medeiro Lima, Sofia Madruga Marcondes Ferraz, Victor Gustavo Kelis Cardoso, Carlos Alberto Teixeira & Leandro Wang Hantao

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  1. Rássius Alexandre Medeiro Lima
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  3. Victor Gustavo Kelis Cardoso
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  4. Carlos Alberto Teixeira
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  5. Leandro Wang Hantao
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Conceptualization, Leandro Wang Hantao; methodology, Carlos Alberto Teixeira, Rássius Alexandre Medeiro Lima, Sofia Madruga Marcondes Ferraz, and Victor Gustavo Kelis Cardoso; formal analysis and investigation, Carlos Alberto Teixeira, Rássius Alexandre Medeiro Lima, Sofia Madruga Marcondes Ferraz, and Victor Gustavo Kelis Cardoso; writing — original draft preparation, Carlos Alberto Teixeira, Rássius Alexandre Medeiro Lima, Sofia Madruga Marcondes Ferraz, and Victor Gustavo Kelis Cardoso; writing — review and editing, Carlos Alberto Teixeira, Leandro Wang Hantao, Rássius Alexandre Medeiro Lima, Sofia Madruga Marcondes Ferraz, and Victor Gustavo Kelis Cardoso; funding acquisition, Leandro Wang Hantao; and supervision, Leandro Wang Hantao.

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Correspondence to Leandro Wang Hantao.

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Lima, R.A.M., Ferraz, S.M.M., Cardoso, V.G.K. et al. Authentication of fish oil (omega-3) supplements using class-oriented chemometrics and comprehensive two-dimensional gas chromatography coupled to mass spectrometry. Anal Bioanal Chem 415, 2601–2611 (2023). https://doi.org/10.1007/s00216-022-04428-2

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