Simultaneous determination of melatonin and 6-hydroxymelatonin in human overnight urine by LC-MS/MS

Article Article scientifique Article Simultaneous determination of melatonin and 6-hydroxymelatonin in human overnight urine by LC-MS/MS eng 2021-09-08 2021-09-01 author Magliocco Gaëlle 0000-0003-4352-5440 752117 author Le Bloc'h Ferdinand 852713 author Thomas Aurélien 647674 author Desmeules Jules Alexandre 73542 author Daali Youssef 46042 122938 10.1016/j.jchromb.2021.122938 34521018 1570-0232 https://www.sciencedirect.com/science/article/pii/S1570023221004190 <p>For the quantification of the pineal hormone melatonin and its metabolite, 6-hydroxymelatonin, in human overnight urine, a single accurate method by liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed. Urine samples were deconjugated using β-glucuronidase/arylsulfatase from <i>Helix pomatia</i> before solid phase extraction (SPE) purification. Chromatographic separation was performed using a reverse phase C18 column with a 7-minute gradient elution. Water was used as matrix to prepare the calibration standards, and deuterated analogues of melatonin and 6-hydroxymelatonin were used as internal standards. This newly developed method was validated in terms of linearity, accuracy, repeatability, intermediate precision, recovery, matrix effect, and stability according to the guidelines of the European Medicines Agency. The method was successfully applied to the analysis of overnight urine samples from 12 healthy volunteers, showing significant correlations of urinary melatonin and 6-hydroxymelatonin excretion rates with age. The urinary 6-hydroxymelatonin to melatonin ratio was also established and will be assessed in further studies as a potential endogenous metric of CYP1A2 activity.</p> CYP450 LC-MS/MS Melatonin Phenotyping Chromatography, Liquid / methods Humans Limit of Detection Linear Models Melatonin / analogs & derivatives Melatonin / urine Reproducibility of Results Solid Phase Extraction Tandem Mass Spectrometry / methods Dewey 615 Dewey 617 Dewey 614.1 31 Section des sciences pharmaceutiques 17 63 Département d'anesthésiologie, pharmacologie, soins intensifs et urgences 229 67 Institut de médecine légale 22A2 false 302 Groupe Desmeules Jules (pharmacologie/toxicologie) 567 1280 Pharmaco-omiques et médecine de précision 1003 Journal of chromatography. B 1181 6a913db6-1220-4e6c-aa2e-7a7428ee1898 Article (Published version) Public 1-s2.0-S1570023221004190-main.pdf 1329380 application/pdf CC BY-NC-ND-4.0 openAccess Faculté des sciences / Section des sciences pharmaceutiques Faculté de médecine / Section de médecine clinique / Département d'anesthésiologie, pharmacologie, soins intensifs et urgences Faculté de médecine / Section de médecine clinique / Département de santé et médecine communautaires / Institut de médecine légale

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Simultaneous determination of melatonin and 6-hydroxymelatonin in human overnight urine by LC-MS/MS	Journal of chromatography. B			2021	437	565

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Le Bloc'h, Ferdinand