title: Mixed silyl ether-perfluoroacyl ester derivatives for gas chromatography/mass spectrometry of oestrogens. Application to the quantitative determination of oestriol in human plasma.
abstract: The conversion of oestrogens into mixed derivatives comprising a phenolic silyl ether and one or more alcoholic perfluoroactyl ester(s) is described. They are easily formed in quantitative yield and have excellent gas chromatographic and mass spectrometric properties, making them suitable for analysis by selected ion monitoring. Reaction mechanisms are examined which propose explanations for the experimentally observed optimal reaction conditions. The 3-t-butyldimethylsilyl ether-16 alpha 17 beta-bis(pentafluoropropionate) has been used for the quantitative determination of oestriol in plasma by gas chromatography/mass spectrometry using a stable isotope internal standard. Comparison with the pertrimethylsilyl ether of oestriol indicates higher specificity and better precision for low-level (less than 0.5 ng ml-1) estimations.
authors.affiliation: Fondation de Recherche en Hormonologie, Fresnes, France.
authors.forename: L
authors.initials: L
authors.lastname: Dehennin
mesh_terms: D002849:Chromatography, Gas; D004952:Esters / Q000032:analysis / Q000138:chemical synthesis; D004964:Estriol / Q000097:blood*; D004967:Estrogens / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D007202:Indicators and Reagents; D013058:Mass Spectrometry; D011865:Radioisotope Dilution Technique; D014297:Trimethylsilyl Compounds / Q000032:analysis
chemical_list: D004952:Esters; D004967:Estrogens; D007202:Indicators and Reagents; D014297:Trimethylsilyl Compounds; D004964:Estriol