A new LC-MS assay for the quantitative analysis of vitamin K metabolites in human urine
| Autor: | Aaron M. Teitelbaum, Catherine K. Yeung, Matthew G. McDonald, Allan E. Rettie, Amanda L. Johnson, Shinya Fujii, Hiroyuki Kagechika |
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| Rok vydání: | 2019 |
| Předmět: |
Adult
Male 0301 basic medicine Vitamin K Metabolite QD415-436 Omega oxidation Urine omega-oxidation 030204 cardiovascular system & hematology Biochemistry beta-oxidation 03 medical and health sciences chemistry.chemical_compound phylloquinone 0302 clinical medicine Endocrinology Tandem Mass Spectrometry Liquid chromatography–mass spectrometry Methods Humans liquid chromatography-mass spectrometry Detection limit Chemical ionization Chromatography Molecular Structure menaquinone Cell Biology Healthy Volunteers 030104 developmental biology chemistry Calibration Dietary Supplements Glucuronide Quantitative analysis (chemistry) Chromatography Liquid |
| Zdroj: | Journal of Lipid Research, Vol 60, Iss 4, Pp 892-899 (2019) |
| ISSN: | 0022-2275 |
| DOI: | 10.1194/jlr.d087916 |
| Popis: | Vitamin K (VK), in both its phylloquinone and menaquinone forms, has been hypothesized to undergo ω- and β-oxidation on its hydrophobic side chain in order to generate the observed urinary metabolites, K acid I and K acid II, which are excreted primarily as glucuronide conjugates. Synthetic standards of K acid I, K acid II, and a putative intermediate metabolite, menaquinone (MK)1 ω-COOH, were used to develop and optimize a new atmospheric pressure negative chemical ionization LC-MS/MS assay for the quantitation of these compounds in urine from untreated individuals and subjects treated with a high dose VK supplement. VK catabolites were extracted from urine, deconjugated, and converted to their methyl ester derivatives using previously reported methodology. The assay showed a high degree of sensitivity, with limits of detection below 10–50 fmol of metabolite per milliliter of urine, as well as an inter-assay precision of 8–12%. Metabolite standards provided unambiguous evidence for MK1 ω-COOH as a new human urinary metabolite of VK. This assay provides a minimally invasive, highly sensitive, and specific alternative for monitoring VK status in humans. |
| Databáze: | OpenAIRE |
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