Methods for quantitative analysis of PGF2 , PGE2, 9 , 11 -dihydroxy-15-keto-prost-5-enoic acid and 9 , 11 , 15-trihydroxy-prost-5-enoic acid from body fluids using deuterated carriers and gas chromatography--mass spectrometry |
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Authors: | K. Gréen E. Granström B. Samuelsson U. Axen |
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Affiliation: | Department of Chemistry, Karolinska Institutet, S-104 01 Stockholm 60, Sweden;Department of Experimental Chemistry, The Upjohn Company, Kalamazoo, Michigan 49001 USA |
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Abstract: | The preparation of (3,3,4,4-D4)-PGE2, (3,3,4,4-D4)-PGF2α, (3,3,4,4-D4)-9α,11α-dihydroxy-15-ketoprost-5-enoic acid and (3,3,4,4-D4)-9α,11α,15-trihydroxyprost-5-enoic acid is described. These compounds have been used for quantitative determination of corresponding nondeuterated prostaglandins by gas-liquid chromatography-mass spectrometry. The method is based on addition of a known amount of carrier to the sample and after purification and derivatization the ratio between the protium and deuterium form is measured in the mass spectrometer. Ions originating in deuterated and nondeuterated molecules are focused one at a time on the electron multiplier using an accelerating voltage alternator.With this technique 400 pg of PGF2α can be determined with a precision of ±3.7% (SD). The recoveries from plasma samples, containing 1–2.5 ng/ml of any of the compounds, is about 100±10%. |
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