Microdetermination of 2,3-dinor-6-ketoprostaglandin F1 alpha in human urine using gas chromatography-high-resolution selected-ion monitoring.
The microdetermination of 2,3-dinor-6-ketoprostaglandin F1 alpha (I) in human urine is described. Samples to which the [2H4]-analogue was added as an internal standard were extracted by chromatographic sample preparation using a Bond Elut C18 cartridge and a silica gel column. Conversion of the extracted I into the 1-methyl ester-6-methoxime-9,11,15-trisdimethylisopropylsilyl ether derivative was followed by gas chromatography-high-resolution selected-ion monitoring (GC-HR-SIM). Interfering substances from the urine matrix were eliminated during GC-HR-SIM analysis using a DB-1 column. A good linear response over the range 10 pg-100 ng per tube was demonstrated. Compound I could be detected in the range 26-375 pg/ml of human urine. The proposed method can be applied to the determination of I in human urine.
Department of Pharmaceutical Sciences, Tohoku University Hospital, Sendai, Japan.
M
M
Mizugaki
T
T
Hishinuma
G S
GS
Yu
K
K
Ito
M
M
Nishikawa
Y
Y
Ohyama
M
M
Ishibashi
Y
Y
Nakagawa
N
N
Harima
D015121:6-Ketoprostaglandin F1 alpha / Q000031:analogs & derivatives* / Q000652:urine; D000293:Adolescent; D000328:Adult; D002138:Calibration; D002849:Chromatography, Gas / Q000379:methods* / Q000706:statistics & numerical data; D005260:Female; D006801:Humans; D006863:Hydrogen-Ion Concentration; D008297:Male; D013058:Mass Spectrometry; D008832:Microchemistry; D008875:Middle Aged; D012016:Reference Values; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
D015121:6-Ketoprostaglandin F1 alpha; C028290:2,3-dinor-6-ketoprostaglandin F1alpha