Journal
MOLECULES
Volume 27, Issue 8, Pages -Publisher
MDPI
DOI: 10.3390/molecules27082427
Keywords
vitamin D; deuterium labeling; liquid-chromatography tandem mass spectrometry; measurement of vitamin D metabolites in blood
Funding
- Japan Agency for Medical Research and Development (AMED- CREST)
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This study describes a versatile method for synthesizing deuterium-labeled D-3 metabolites and successfully applies it to measure the concentration of these compounds in pooled human serum. This includes the first quantification of 1,25(OH)(2)D-3-23,26-lactone in human serum.
Blood levels of the vitamin D-3 (D-3) metabolites 25-hydroxyvitamin D-3 (25(OH)D-3), 24R,25-dihydroxyvitamin D-3, and 1 alpha,25-dihydroxyvitamin D-3 (1,25(OH)(2)D-3) are recognized indicators for the diagnosis of bone metabolism-related diseases, D-3 deficiency-related diseases, and hypercalcemia, and are generally measured by liquid-chromatography tandem mass spectrometry (LC-MS/MS) using an isotope dilution method. However, other D-3 metabolites, such as 20-hydroxyvitamin D-3 and lactone D-3, also show interesting biological activities and stable isotope-labeled derivatives are required for LC-MS/MS analysis of their concentrations in serum. Here, we describe a versatile synthesis of deuterium-labeled D-3 metabolites using A-ring synthons containing three deuterium atoms. Deuterium-labeled 25(OH)D-3 (2), 25(OH)D-3-23,26-lactone (6), and 1,25(OH)(2)D-3-23,26-lactone (7) were synthesized, and successfully applied as internal standards for the measurement of these compounds in pooled human serum. This is the first quantification of 1,25(OH)(2)D-3-23,26-lactone (7) in human serum.
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