title: Novel derivatization and immunoextraction to improve microanalysis of 11-dehydrothromboxane B2 in human urine.
abstract: A new, highly selective procedure for the determination of 11-dehydrothromboxane B2 (11-dehydro-TXB2) in human urine is described. Following the addition of [19,19,20,20-2H4]11-dehydro-TXB2 as an internal standard, samples were extracted with an affinity column of anti-11-dehydro-TXB2. Conversion of the immunoextracted 11-dehydro-TXB2 into its 1-methyl ester-11-n-propylamide-9,12,15-tris-dimethylisopropylsilyl ether derivative was followed by gas chromatography-selected-ion monitoring. The mass spectrum of the 11-dehydro-TXB2 derivative was dominated by the base peak ion of [M-C3H7]+ at m/z 698, which accounted for more than 10% of the total ion current. A typical result showed that the immunoaffinity purification procedures provided an extremely clean alternative to more conventional methods of chromatographic fractionation, and that interfering substances from the urine matrix were almost entirely eliminated during the microanalysis.
authors.affiliation: Research Laboratories, Nippon Kayaku Co. Ltd., Tokyo, Japan.
authors.forename: M
authors.initials: M
authors.lastname: Ishibashi
authors.forename: K
authors.initials: K
authors.lastname: Watanabe
authors.forename: Y
authors.initials: Y
authors.lastname: Ohyama
authors.forename: M
authors.initials: M
authors.lastname: Mizugaki
authors.forename: Y
authors.initials: Y
authors.lastname: Hayashi
authors.forename: W
authors.initials: W
authors.lastname: Takasaki
mesh_terms: D000911:Antibodies, Monoclonal; D002849:Chromatography, Gas; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D007202:Indicators and Reagents; D008832:Microchemistry; D011863:Radioimmunoassay; D012015:Reference Standards; D013929:Thromboxane B2 / Q000031:analogs & derivatives* / Q000276:immunology / Q000652:urine
chemical_list: D000911:Antibodies, Monoclonal; D007202:Indicators and Reagents; D013929:Thromboxane B2; C049235:11-dehydro-thromboxane B2