Gas chromatographic-mass spectrometric determination of 11-dehydrothromboxane B2 in human urine.
The extension of a method for the determination of thromboxane B2 (TxB2), 2,3-dinor-TxB2, 6-keto-prostaglandin F1 alpha (6-keto-PGF1 alpha) and 2,3-dinor-6-keto-PGF1 alpha to quantify 11-dehydro-TxB2 in the same urinary sample is described. After phenylboronic acid and C18 column chromatography, 11-dehydro-TxB2, which is present in urine as the lactone and its corresponding hydroxy acid, was quantitatively converted into its lactone form for a thin-layer purification step and pentafluorobenzyl esterification. Quantification of eicosanoids was achieved by analysing their trimethylsilyl ethers with gas chromatography and negative-ion chemical ionization mass spectrometry. The overall recovery from urine for tritiated 11-dehydro-TxB2 was 80%. The detection limit was 10 pg/ml. The method was applied to the determination of these eicosanoids in volunteers and in patients suffering from acute myocardial infarction.
Weber
C
C
Janssen Research Foundation, Neuss, Germany.
Beetens
J
J
De Clerck
F
F
Tegtmeier
F
F
D002855:Chromatography, Thin Layer; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D008297:Male; D009203:Myocardial Infarction / Q000652:urine; D015203:Reproducibility of Results; D013929:Thromboxane B2 / Q000031:analogs & derivatives* / Q000652:urine
D013929:Thromboxane B2; C049235:11-dehydro-thromboxane B2