Determination of 22-oxacalcitriol, a new analog of 1alpha,25-dihydroxyvitamin D3, in human serum by liquid chromatography-mass spectrometry

Journal of Chromatography. B, Biomedical Sciences and Applications
Masaki IshigaiK Kumaki

Abstract

A sensitive and specific liquid chromatographic-mass spectrometric assay has been developed for the determination of 22-oxacalcitriol (OCT), which is a new analog of 1alpha,25-dihydroxyvitamin D3. The analyte was isolated from serum by two solid-phase extraction steps on a C18 cartridge and NH2 cartridge. The recovery of OCT through two extraction steps was more than 90%. A related substance (ED-94), i.e. OCT with the side-chain shortened by one carbon, was used as an internal standard. Extracts were chromatographed on a C18 reversed-phase column interfaced to the electrospray ionization source. The mass spectrometer was operated in the positive-ion mode of selected reaction monitoring. The chromatographic run-time for one injection was less than 6 min. The intra- and inter-assay coefficients of variation for the lowest concentration examined (30 pg ml[-1]) were 9.83 and 10.67, respectively. And the analytical recovery of OCT added to serum was quantitative. Assay linearity was obtained in the range of 20-640 pg ml(-1).

Citations

Mar 27, 2004·European Journal of Pharmacology·Shuichi TsuruokaAkio Fujimura
May 15, 2002·Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences·Tatsuya HigashiKazutake Shimada
Nov 4, 2004·British Journal of Clinical Pharmacology·Shuichi TsuruokaAkio Fujimura
Aug 17, 2005·Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences·Naoaki MuraoYoshinori Aso
Dec 3, 2004·Journal of the American Society of Nephrology : JASN·Kazuhiro ShiizakiTadao Akizawa
Nov 26, 2005·Bioorganic & Medicinal Chemistry·Kazuki ShimizuKazumi Morikawa

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