title: Microdetermination of the 6,15-diketo-13,14-dihydroprostaglandin F1alpha in human plasma using gas chromatography/selected ion monitoring with [18O]6,15-diketo-13,14-dihydro-prostaglandin F1alpha as an internal standard.
abstract: We devised a simple and effective purification method for the microdetermination of 6,15-diketo-13,14-dihydro-prostaglandin F1alpha (DK), a metabolite of prostacyclin (PGI2). [18O]DK was synthesized from the repeated base-catalyzed hydrolysis of methyl ester derivatives in [18O] water to obtain an internal standard for the gas chromatography/selected ion monitoring (GC/SIM) of DK. The methyl ester-methoxime-tert-butyldimethylsilyl ether derivative was prepared, then gas chromatography/selected ion monitoring was carried out by monitoring the ion at m/z 613.4 for DK and at m/z 617.4 for an internal standard. A good linear response over the range of 10 pg to 10 ng was demonstrated. We detected DK to a level of about 297.8 pg/ml in human plasma. This method can be used to determine DK in biological samples.
authors.affiliation: Department of Pharmaceutical Sciences, Tohoku University Hospital, Sendai, Japan. mizugaki@mail.cc.tohoku.ac.jp
authors.forename: M
authors.initials: M
authors.lastname: Mizugaki
authors.forename: T
authors.initials: T
authors.lastname: Hishinuma
authors.forename: H
authors.initials: H
authors.lastname: Yamaguchi
authors.forename: K
authors.initials: K
authors.lastname: Kanno
authors.forename: Y
authors.initials: Y
authors.lastname: Hirose
authors.forename: H
authors.initials: H
authors.lastname: Nakamura
mesh_terms: D015121:6-Ketoprostaglandin F1 alpha / Q000031:analogs & derivatives* / Q000032:analysis / Q000097:blood / Q000592:standards; D000328:Adult; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D006801:Humans; D010103:Oxygen Isotopes; D012015:Reference Standards; D012680:Sensitivity and Specificity; D012821:Silanes / Q000737:chemistry
chemical_list: D010103:Oxygen Isotopes; D012821:Silanes; D015121:6-Ketoprostaglandin F1 alpha; C033371:6,15-diketo-13,14-dihydroprostaglandin F1alpha