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Comparison of Analytical Methods for the Rapid Determination of Melatonin in Food Supplements

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Abstract

Melatonin is a hormone produced by the pineal gland and extra-pineal tissues with chronobiotic effects that can alter the circadian rhythms, among other health benefits. This study intended to compare two different methods, high-performance liquid chromatography coupled to a variable wavelength detector plus a fluorescence detector (HPLC-VWD-FLD) and constant-wavelength synchronous spectrofluorimetry, to determine melatonin in food supplements. HPLC-MS/MS was used as a confirmatory technique. The data showed that both analytical methodologies were valid for the determination of melatonin with correlation between the datasets obtained (99% confidence level). Constant-wavelength synchronous spectrofluorimetry is a fast, simple, and economical method that can be used for a rapid and precise determination of melatonin in supplements, in the absence of other compounds that could interfere in the analysis. On the other hand, the HPLC-VWD-FLD method showed to be more suitable for the determination of melatonin in complex samples because of its high sensitivity and separation efficiency. Finally, all supplements analyzed from the Spanish market comply with the melatonin content declared on the label and with the claim “contributes to the alleviation of subjective feelings of the jet lag of jet lag” (0.5 mg/day). Also, 7 out of 10 complain about the claim “contributes to the reduction of time taken to fall asleep” (1 mg/day).

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Abbreviations

HPLC-VWD-FLD:

High-performance liquid chromatography coupled to a variable wavelength detector plus a fluorescence detector

HPLC-MS/MS:

High-performance liquid chromatography tandem mass spectrometry

ELISA:

Enzyme-linked immunosorbent assay

GC-MS:

Gas chromatography coupled to mass spectrometry

RIA:

Radioimmunoassay

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Acknowledgements

L. Barbosa-Pereira is grateful to the Spanish Ministry of Science, Innovation and Universities for her “Juan de la Cierva–Incorporación” Grant (agreement No. IJCI-2017-31665).

Funding

This research was financially supported by “Consellería de Cultura, Educación e Ordenación Universitaria, Xunta de Galicia”, ref. No. GRC 2019/030.

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Authors

Contributions

S. Barreiro Astray: Methodology, investigation, and writing—original draft. L. Barbosa-Pereira: Writing—original draft, and writing—review and editing. M.A. Lage-Yusty: Conceptualization, supervision, writing—review and editing, resources, and project administration. J. López-Hernández: Conceptualization, supervision, writing—original draft, resources, and project administration.

Corresponding author

Correspondence to Letricia Barbosa-Pereira.

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Conflict of Interest

Sandra Barreiro Astray declares that she has no conflict of interest. Letricia Barbosa-Pereira declares that she has no conflict of interest. María Asunción Lage-Yusty declares that he has no conflict of interest. Julia López-Hernández declares that she has no conflict of interest.

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Barreiro Astray, S., Barbosa-Pereira, L., Lage-Yusty, M.A. et al. Comparison of Analytical Methods for the Rapid Determination of Melatonin in Food Supplements. Food Anal. Methods 14, 734–741 (2021). https://doi.org/10.1007/s12161-020-01912-2

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  • DOI: https://doi.org/10.1007/s12161-020-01912-2

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