title: Quantitative liquid chromatography-tandem mass spectrometric analysis of 11-dehydro TXB2 in urine.
abstract: A simple and selective determination method of 11-dehydrothromboxane B2 (11-dehydroTXB2), which is urinary metabolite of TXA2, has been developed employing liquid chromatography-tandem mass spectrometry (LC-MS-MS). 11-DehydroTXB2 and its deuterium-labeled analogue as an internal standard were extracted from urine by simple solid-phase extraction (SPE). These compounds were analyzed using LC-MS-MS in the selected reaction monitoring (SRM) mode, by monitoring the transitions from m/z 367 to m/z 161 for 11-dehydroTXB2 and from m/z 371 to m/z 165 for its internal standard. A good linear response over the range 50 pg-10 ng per tube was demonstrated. The values determined by LC-MS-MS were well validated and closely corresponded to the values determined by gas chromatography-mass spectrometry (GC-MS). The mean concentration of 11-dehydroTXB2 in urine of healthy adults was 635 +/- 427 pg/mg creatinine (mean +/- S.D., n = 13). This simple, accurate and selective determination method described in this study should greatly aid in evaluating the role of TXA2 in vivo.
authors.affiliation: Department of Pharmaceutical Sciences, Tohoku University Hospital, 1-1 Seiryo-machi, Aoba-ku, Sendai 980-8574, Japan.
authors.forename: Naoto
authors.initials: N
authors.lastname: Suzuki
authors.forename: Takanori
authors.initials: T
authors.lastname: Hishinuma
authors.forename: Satoko
authors.initials: S
authors.lastname: Chiba
authors.forename: Toshihide
authors.initials: T
authors.lastname: Saga
authors.forename: Hiroki
authors.initials: H
authors.lastname: Tsukamoto
authors.forename: Michinao
authors.initials: M
authors.lastname: Mizugaki
authors.forename: Junichi
authors.initials: J
authors.lastname: Goto
mesh_terms: D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003404:Creatinine / Q000652:urine; D005260:Female; D006801:Humans; D008297:Male; D011237:Predictive Value of Tests; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013048:Specimen Handling; D018629:Spectrometry, Mass, Secondary Ion / Q000379:methods*; D013928:Thromboxane A2 / Q000378:metabolism*; D013929:Thromboxane B2 / Q000031:analogs & derivatives* / Q000652:urine*
chemical_list: D013929:Thromboxane B2; D013928:Thromboxane A2; C049235:11-dehydro-thromboxane B2; D003404:Creatinine