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Direct derivatization of sulphate esters for analysis by gas chromatography mass spectrometry
Author(s) -
Murray Stephen,
Baillie Thomas A.
Publication year - 1979
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.1200060209
Subject(s) - trifluoroacetic anhydride , derivatization , chemistry , mass spectrometry , gas chromatography–mass spectrometry , reagent , chromatography , gas chromatography , phenol , yield (engineering) , alicyclic compound , organic chemistry , materials science , metallurgy
Gas chromatography mass spectrometry has been used to study the reaction between a range of aromatic, alicyclic and aliphatic sulphate esters and three perfluoroacylating reagents, viz. trifluoroacetic, pentafluoropropionic and heptafluorobutyric anhydride. Aromatic sulphates were found to react readily, when treated with a 1:1 mixture of a perfluoroacid anhydride and dry ethyl acetate, to form the perfluoroester derivative of the parent phenol in quantitative yield. Non‐aromatic sulphates, on the other hand, gave a variety of products. A mechanism is proposed for the one‐step derivatization of aromatic sulphates and the potential of the procedure for the analysis of sulphate conjugates by mass spectrometry is discussed.