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.
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.
Mizugaki
M
M
Department of Pharmaceutical Sciences, Tohoku University Hospital, Sendai, Japan. mizugaki@mail.cc.tohoku.ac.jp
Hishinuma
T
T
Yamaguchi
H
H
Kanno
K
K
Hirose
Y
Y
Nakamura
H
H
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
D010103:Oxygen Isotopes; D012821:Silanes; D015121:6-Ketoprostaglandin F1 alpha; C033371:6,15-diketo-13,14-dihydroprostaglandin F1alpha