Mixed silyl ether–perfluoroacyl ester derivatives for gas chromatography/mass spectrometry of oestrogens. Application to the quantitative determination of oestriol in human plasma

✍ Scribed by L. Dehennin

• Publisher: John Wiley and Sons
• Year: 1989
• Tongue: English
• Weight: 480 KB
• Volume: 18
• Category: Article
• ISSN: 1076-5174
• DOI: 10.1002/bms.1200180506

✦ Synopsis

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 chromate graphic 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-1óal7~bis(pentafluoropropionate) has been used for the quantitative determination of oestriol in plasma by gas chromatography/mass spectrometry using a stable isotope interna1 standard.

Comparison with the pertrimethylsilyl ether of oestriol indicates higher specificity and better precision for low-leve1 (< 0.5 ng ml-') estimations. Receiued I I Au(gu.\t IYXX Reivsed 30 Ocrober 1988 Oestrogen E-3.1 7B-di0l (oestradiolLl7fl) E-3.1 7o-di0l (oestradiol-l7a) E-2,3,17/3-triol E-2-rnethoxy-3,17/3-diol E-3.1 6a,l7/3-triol (oestriol) Major ions abovemlz 200 (with Derivative Retention index relative abundances)