Microdetermination of 11-dehydrothromboxane B2 in human urine by gas chromatography-selected-ion monitoring.
Simple and effective purification for quantitation of trace amounts of 11-dehydrothromboxane B2 (11-dehydro-TXB2) in human urine by gas chromatography-selected-ion monitoring (GC-SIM) was achieved. The procedure is based on stepwise elution of the methyl ester derivative from a silica gel column with n-hexane-ethyl acetate (1:1) after washing the column with n-hexane-ethyl acetate (2:1). After the methyl ester has been converted into the corresponding dimethylisopropylsilyl ether, GC-SIM is carried out by monitoring the ion at m/z 539.32 for 11-dehydro-TXB2 and that at m/z 543.33 for its 18O2-labelled variant as an internal standard. The detection limit is 2 pg per injection with a signal-to-noise ratio of 5:1. The method was applied to the determination of 11-dehydro-TXB2 in human urine.
Watanabe
K
K
Research Laboratories, Pharmaceuticals Group, Nippon Kayaku Co., Tokyo, Japan.
Yamashita
K
K
Ishibashi
M
M
Hayashi
Y
Y
Yamamoto
S
S
Miyazaki
H
H
D055598:Chemical Phenomena; D002621:Chemistry; D002849:Chromatography, Gas / Q000379:methods; D002851:Chromatography, High Pressure Liquid; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D013929:Thromboxane B2 / Q000031:analogs & derivatives* / Q000652:urine
D013929:Thromboxane B2; C049235:11-dehydro-thromboxane B2