Determination of urinary prostanoids by capillary gas chromatography/high-resolution mass spectrometry |
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Authors: | David A Herold John Savory Michael Kinter Richard Ross Michael R Wills |
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Institution: | Departments of Pathology, Biochemistry and Internal Medicine, University of Virginia Medical Center, Charlottesville, VA 22908 U.S.A. |
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Abstract: | A stable isotope-dilution gas-chromatography/high-resolution mass spectrometry method for the determination of prostaglandin E2 (PGE2) and 6-keto-prostaglandin F1α (6-keto-PGF1α) in urine as their methoxime/t-butyldimethylsilyl ether/t-butyl-dimethylsilyl ester derivatives is described. The derivatives are prepared by a novel derivatization scheme in which the pentafluorobenzyl esters are formed prior to the silylation step in which the t-butyldimethylsilyl esters are formed in an apparent exchange reaction. Recoveries through the entire extraction and derivatization procedure are 70.6% for PGE2 and 64.4% for 6-keto-PGF1α. Quantitation at mass resolutions approaching 10 000 eliminated all interferences in the PGE2 chromatograms while lower resolutions were sufficient for 6-keto-PGF1α. Limits of detection of 50 pg ml?1 for each prostanoid were obtained. For PGE2, a lower limit of detection was obtained at a mass resolution of 10 000 (50 pg ml?1) than was obtained at a mass resolution of 1000 (80 pg ml?1), illustrating the selectivity of detection. |
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