title: 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.
abstract: 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.
authors.affiliation: Research Laboratories, Nippon Kayaku Co., Ltd., Tokyo, Japan.
authors.forename: M
authors.initials: M
authors.lastname: Ishibashi
authors.forename: Y
authors.initials: Y
authors.lastname: Nakagawa
authors.forename: N
authors.initials: N
authors.lastname: Harima
authors.forename: T
authors.initials: T
authors.lastname: Hishinuma
authors.forename: M
authors.initials: M
authors.lastname: Mizugaki
mesh_terms: 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
chemical_list: D007202:Indicators and Reagents; D010103:Oxygen Isotopes; D013929:Thromboxane B2; C049235:11-dehydro-thromboxane B2