| The determination of 2beta-(3-hydroxypropoxy)-1alpha,25-dihydroxy vitamin D3 (ED-71) in human serum by high-performance liquid chromatography-electrospray tandem mass spectrometry. | |
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MedLine Citation:
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PMID: 16102526 Owner: NLM Status: MEDLINE |
Abstract/OtherAbstract:
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A liquid chromatography-electrospray ionization tandem mass spectrometric (LC/ESI-MS/MS) method for the determination of 2beta-(3-hydroxypropoxy)-1alpha,25-dihydroxy vitamin D3 (ED-71) in human serum has been developed. ED-71 in human serum was extracted using two solid-phase extraction steps on Bond Elut C18 and NH2 cartridge. The separation of ED-71 and preED-71 isomer was attained by LC using 2 mmol/L ammonium acetate-methanol (15:85, v/v) as a mobile phase on a Symmetry C18 column (5 microm, 150 mm x 2.1mm i.d.). ESI-MS/MS analysis was operated using selected reaction monitoring (SRM) in positive ion mode. The method achieved a lower limit of quantitation of 25 pg/mL. The calibration curve (25-3200 pg/mL) gave acceptable linearity (r>0.9964). Intra-assay precision ranged from 2.3 to 9.7%. Inter-assay precision ranged from 1.0 to 3.4%. The accuracy was within 90.8-107.0%. This highly sensitive and reproducible method is able to determine only biologically active ED-71 by separating it from preED-71, which is considered to be applicable for the determination of serum samples from pharmacokinetic studies in human. |
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Authors:
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Naoaki Murao; Norihisa Ohishi; Yoshiaki Nabuchi; Masaki Ishigai; Takehiko Kawanishi; Yoshinori Aso |
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Publication Detail:
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Type: Comparative Study; Journal Article Date: 2004-11-19 |
Journal Detail:
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Title: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Volume: 823 ISSN: 1570-0232 ISO Abbreviation: J. Chromatogr. B Analyt. Technol. Biomed. Life Sci. Publication Date: 2005 Sep |
Date Detail:
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Created Date: 2005-08-16 Completed Date: 2005-09-21 Revised Date: 2006-11-15 |
Medline Journal Info:
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Nlm Unique ID: 101139554 Medline TA: J Chromatogr B Analyt Technol Biomed Life Sci Country: Netherlands |
Other Details:
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Languages: eng Pagination: 61-8 Citation Subset: IM |
Affiliation:
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Fuji Gotemba Research Laboratories, Chugai Pharmaceutical Company Ltd., 1-135 Komakado, Gotemba, Shizuoka 412-8513, Japan. muraonoa@chugai-pharm.co.jp |
Export Citation:
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| MeSH Terms | |
Descriptor/Qualifier:
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Calcitriol
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analogs & derivatives*,
blood Calibration Chromatography, High Pressure Liquid / methods* Humans Reproducibility of Results Spectrometry, Mass, Electrospray Ionization / methods* Temperature Time Factors |
| Chemical | |
Reg. No./Substance:
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104121-92-8/2-(3-hydroxypropoxy)-1,25-dihydroxyvitamin D3; 32222-06-3/Calcitriol |
From MEDLINE®/PubMed®, a database of the U.S. National Library of Medicine
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