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Quantitative determination of F 6 ‐1,25(OH) 2 vitamin D 3 in human serum by gas chromatography/mass spectrometry with high‐resolution selected ion monitoring
Author(s) -
Komuro Setsuko,
Nakatsuka Iwao,
Yoshitake Akira,
Iba Kazuhiko
Publication year - 1994
Publication title -
biological mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.475
H-Index - 121
eISSN - 1096-9888
pISSN - 1052-9306
DOI - 10.1002/bms.1200230107
Subject(s) - chromatography , chemistry , mass spectrometry , resolution (logic) , selected ion monitoring , detection limit , gas chromatography , extraction (chemistry) , gas chromatography–mass spectrometry , vitamin , biochemistry , artificial intelligence , computer science
A highly sensitive and specific gas chromatographic/mass spectrometric method was developed for the determination of very low levels of F 6 ‐1,25(OH) 2 vitamin D 3 , a new fluoro analogue of vitamin D 3 , to facilitate investigation of its pharmacokinetics in man. Deuterium‐labelled F 6 ‐1,25(OH) 2 vitamin D 3 was employed as an internal standard for quantification. The method involves extraction from serum samples, separation by a cartridge column system followed by straight‐phase high‐performance liquid chromatography, O ‐trimethylsilylation, and analysis by gas chromatography/mass spectrometry using high‐resolution selected ion monitoring. With a quantification limit of 2 pg ml −1 and a requirement for 2 ml of serum, the assay method has sufficient sensitivity, selectivity and precision for the analysis of very low concentrations of the drug.