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J Chromatogr B Biomed Sci Appl. 1997 Dec 19;704(1-2):11-7.

Characteristics of mass spectrometric analyses coupled to gas chromatography and liquid chromatography for 22-oxacalcitriol, a vitamin D3 analog, and related compounds.

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Drug Metabolism and Pharmacokinetics Research Laboratory, Chugai Pharmaceutical Co. Ltd., Tokyo, Japan.


The characteristics of the mass spectra of vitamin D3 related compounds were investigated by GC-MS and LC-MS using 22-oxacalcitriol (OCT), an analog of 1,25-dihydroxyvitamin D3, and related compounds. Fragmentation during GC-MS (electron impact ionization) of TMS-derivatives of OCT and the postulated metabolites gave useful structural information concerning the vitamin D3-skeleton and its side-chain, especially with respect to the oxidation positions of metabolites. In contrast, few fragment ions were observed in LC-MS (atmospheric pressure chemical ionization), showing that LC-MS gave poor structural information, except for molecular mass. However, when comparing the signal-to-noise ratio (S/N) observed during GC-MS and LC-MS analysis for OCT in plasma extracts, the S/N in LC-MS was over ten-times greater than in GC-MS, possibly due to the low recovery on derivatization and thermal-isomerization in GC-MS. Furthermore, both the GC-MS and the LC-MS allowed the analysis of many postulated metabolites in a single injection without any prior isolation of target metabolites from biological fluids by LC. These results suggest that GC-MS and LC-MS analysis for vitamin D3 related compounds such as OCT each have unique and distinct advantages. Therefore, the complementary use of both techniques enables the rapid and detailed characterization of vitamin D3 related compounds.

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