Comparison of Analytical Methods for the Rapid Determination of Melatonin in Food Supplements
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Comparison of Analytical Methods for the Rapid Determination of Melatonin in Food Supplements Sandra Barreiro Astray 1 & Letricia Barbosa-Pereira 1
&
María Asunción Lage-Yusty 1 & Julia López-Hernández 1
Received: 29 April 2020 / Accepted: 1 November 2020 # Springer Science+Business Media, LLC, part of Springer Nature 2020
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). Keywords Melatonin . Circadian rhythms . Food supplements . High-performance liquid chromatography . Spectrofluorimetry
Abbreviations HPLC-VWD-FLD
HPLC-MS/MS
ELISA GC-MS RIA
Introduction High-performance liquid chromatography coupled to a variable wavelength detector plus a fluorescence detector High-performance liquid chromatography tandem mass spectrometry Enzyme-linked immunosorbent assay Gas chromatography coupled to mass spectrometry Radioimmunoassay
* Letricia Barbosa-Pereira [email protected] 1
Department of Analytical Chemistry, Nutrition and Food Science, Faculty of Pharmacy, University of Santiago de Compostela, Campus Vida, 15782 Santiago de Compostela, Spain
Melatonin (N-acetyl-5-methoxytryptamine) is a neurohormone synthesized from the amino acid tryptophan in the pineal gland (Kocadăgli et al. 2014). The main interest of this indolamine is related to its many beneficial functions to human health and well-being. The chemical structure of Nacetyl-5-methoxytryptamine (Fig. 1) consists of an indolic ring and two main functional groups, the amide group in position 3 and the methoxy group in position 5, that determine its amphipathic character. This property confers it the ability to cross membranes, thus reaching cellular compartments such a
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