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Simultaneous determination of 6‐oxo‐prosta‐glandin F 1α and 2,3‐dinor‐6‐oxo‐prostaglandin F 1α in biological fluids by stable isotope dilution and negative ion chemical ionization mass spectrometry
Author(s) -
Fischer C.,
Meese C. O.
Publication year - 1985
Publication title -
biomedical mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.475
H-Index - 121
eISSN - 1096-9888
pISSN - 0306-042X
DOI - 10.1002/bms.1200120808
Subject(s) - chemistry , metabolite , chemical ionization , isotope dilution , chromatography , mass spectrometry , trimethylsilyl , ether , detection limit , prostaglandin d2 , derivatization , urine , selected reaction monitoring , prostaglandin , ionization , ion , tandem mass spectrometry , medicinal chemistry , biochemistry , organic chemistry
A stable isotope dilution assay for the simultaneous determination of two metabolites of prostacyclin (1), 6‐oxoprostaglandin F 1α (2a) and 2,3‐dinor‐6‐oxo‐prostaglandin F 1α (3a), in human seminal fluid and human urine is described. A new chemical total synthesis of deuterated internal standard, 18,18,19,19‐( 2 H 4 )‐2,3‐dinor‐6‐oxo‐PGF 1α (3b), is presented and enables specific and sensitive quantification based on negative ion chemical ionization mass spectrometry. 2a and 3a were analysed as their methoxime pentafluorobenzyl ester tris(trimethylsilyl) ether derivatives in the selected ion monitoring mode registrating the [M‐181] − fragments with a detection limit for both prostanoids of 10 pg per injection. The two metabolites occur in human seminal fluid in very low concentrations (2a: 2.8 ng ml −1 ; 3a: 1.7 ng ml −1 ) and cannot contribute significantly to the urinary metabolite levels which are in the range of 108‐265 ng/24 h for 3a and 124‐574 ng/24 h for 2a.