Quantitative determination of F6-1,25(OH)2 vitamin D3 in human serum by gas chromatography/mass spectrometry with high-resolution selected ion monitoring.
A highly sensitive and specific gas chromatographic/mass spectrometric method was developed for the determination of very low levels of F6-1,25(OH)2 vitamin D3, a new fluoro analogue of vitamin D3, to facilitate investigation of its pharmacokinetics in man. Deuterium-labelled F6-1,25(OH)2 vitamin D3 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.
Komuro
S
S
Environmental Health Science Laboratory, Sumitomo Chemical Co., Ltd, Osaka, Japan.
Nakatsuka
I
I
Yoshitake
A
A
Iba
K
K
D002117:Calcitriol / Q000031:analogs & derivatives* / Q000097:blood / Q000493:pharmacokinetics; D002851:Chromatography, High Pressure Liquid; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D006207:Half-Life; D006801:Humans; D007553:Isotope Labeling; D013056:Spectrophotometry, Ultraviolet; D005466:Fluorocarbons
D002117:Calcitriol; C040488:26,26,26,27,27,27-hexafluoro-1,25-dihydroxyvitamin D3; D005466:Fluorocarbons