ANALYSIS OF 11-DEHYDROTHROMBOXANE B-2 IN HUMAN URINE IMPROVED BY USE OF GAS-CHROMATOGRAPHY HIGH-RESOLUTION SELECTED-ION MONITORING WITH O-18(2)-LABELED ANALOG AS AN INTERNAL STANDARD
M. Ishibashi et al., ANALYSIS OF 11-DEHYDROTHROMBOXANE B-2 IN HUMAN URINE IMPROVED BY USE OF GAS-CHROMATOGRAPHY HIGH-RESOLUTION SELECTED-ION MONITORING WITH O-18(2)-LABELED ANALOG AS AN INTERNAL STANDARD, Biological mass spectrometry, 23(10), 1994, pp. 612-620
Gas chromatography/high-resolution selected ion monitoring (GC/HR-SIM)
for the determination of 11-dehydrothromboxane B-2 (11-dehydro-TXB(2)
) in human urine is described, Combined use of the lactone ring openin
g reaction and dimethylisopropylsilylation has been adopted for the an
alysis of 11-dehydro-TXB(2), to give a new chemically stable derivativ
e. The feasibility of using this derivative for the analysis of 11-deh
ydro-TXB(2) in human urine has been evaluated. Following the addition
of O-18(2)-labelled analogue, for use as an internal standard, the sam
ples were extracted using chromatographic separation with Bond Elut C-
18 and silica gel. Derivatization of the extracted 11-dehydro-TXB(2) w
as followed by GC/SIM at resolution of 5000. This method enables selec
tive detection of 11-dehydro-TXB(2) in human urine without serious int
erference from other endogenous substances. In 11 volunteers, the mean
urinary excretions of 11-dehydro-TXB(2) was 547.6 +/- 217.6 ng per da
y.