Measurement of urinary 2,3-dinor-thromboxane B2 and thromboxane B2 using bonded-phase phenylboronic acid columns and capillary gas chromatography--negative-ion chemical ionization mass spectrometry.
The use of bonded-phase phenylboronic acid columns to selectively extract 2,3-dinor-thromboxane B2 and thromboxane B2 from urine is reported. The compounds were first derivatized as the methoxime and then applied to the phenylboronic acid columns. Subsequent purification by thin-layer chromatography and derivatization to the pentafluorobenzyl ester, trimethylsilyl ether followed by capillary gas chromatography-negative-ion chemical ionization mass spectrometry, monitoring specific ions, allows quantitation in the low-picogram/milliliter range. In healthy male volunteers, the median excretions of 2,3-dinor-thromboxane B2 and thromboxane B2 were 10.3 ng/h (range, 4.5-24 ng/h) and 2.8 ng/h (range, 0.5-7.3 ng/h), respectively. The method offers a noninvasive, specific approach to the study of thromboxane synthesis and platelet function in man. It is much less labor intensive than currently available methods employing electron-impact chromatography-mass spectrometry.
D001897:Boronic Acids; D004563:Electrochemistry; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D006801:Humans; D008297:Male; D012997:Solvents; D013929:Thromboxane B2 / Q000031:analogs & derivatives* / Q000652:urine*
D001897:Boronic Acids; D012997:Solvents; D013929:Thromboxane B2; C028965:2,3-dinor-thromboxane B2; C010686:benzeneboronic acid