Analysis of 11-dehydrothromboxane B2 in human urine improved by use of gas chromatography/high-resolution selected ion monitoring with 18O2-labelled analogue as an internal standard.
Gas chromatography/high-resolution selected ion monitoring (GC/HR-SIM) for the determination of 11-dehydrothromboxane B2 (11-dehydro-TXB2) in human urine is described. Combined use of the lactone ring opening reaction and dimethylisopropylsilylation has been adopted for the analysis of 11-dehydro-TXB2, to give a new chemically stable derivative. The feasibility of using this derivative for the analysis of 11-dehydro-TXB2 in human urine has been evaluated. Following the addition of 18O2-labelled analogue, for use as an internal standard, the samples were extracted using chromatographic separation with Bond Elut C18 and silica gel. Derivatization of the extracted 11-dehydro-TXB2 was followed by GC/SIM at resolution of 5000. This method enables selective detection of 11-dehydro-TXB2 in human urine without serious interference from other endogenous substances. In 11 volunteers, the mean urinary excretions of 11-dehydro-TXB2 was 547.6 +/- 217.6 ng per day.
Ishibashi
M
M
Research Laboratories, Nippon Kayaku Co., Ltd., Tokyo, Japan.
Nakagawa
Y
Y
Harima
N
N
Hishinuma
T
T
Mizugaki
M
M
D002849:Chromatography, Gas; D007202:Indicators and Reagents; D010103:Oxygen Isotopes; D012015:Reference Standards; D018629:Spectrometry, Mass, Secondary Ion; D013929:Thromboxane B2 / Q000031:analogs & derivatives* / Q000652:urine
D007202:Indicators and Reagents; D010103:Oxygen Isotopes; D013929:Thromboxane B2; C049235:11-dehydro-thromboxane B2