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A. Nagl, R. Durán Outeiral, E. Rosenberg:
"Method Development for The Analysis of Acidic PAH Metabolites by GC/MS after TMSH Derivatisation";
Poster: 36th International Symposium on Capillary Chromatography (36th ISCC), Riva del Garda, Italy; 27.05.2012 - 01.06.2012.

A convenient method has been developed for the quantitative analysis of acidic PAH metabolites in water and aqueous environmental samples. The method is based on liquid/liquid extraction of the acidic metabolites (various naphthalene and methyl-naphthalene carboxylic acids, fluorene-9-carboxylic acid, 5-acenaphtene carboxylic acid, some tetrahydro-naphthoic acids and 1-naphthyl acetic acid), followed by derivatization by TMSH (= tetramethyl sulfonium hydroxide). The method leads to the quantitative conversion of the PAH acids into their methyl esters which are detected by GC/MS. Calibration and detection of the target analytes in the SIM mode provided detection limits in the range of 0.02-0.06 μg/L with quantitation limits typically being a factor of ca. three higher. After optimisation of the individual parameters of the sample preparation procedure, the method was validated and applied to the analysis of surface water samples to demonstrate the usability of this approach.
While satisfactory recoveries were confirmed with spiked samples, no acidic PAH metabolites were detected at concentrations above the LOQ. The developed method will in he future be used for more comprehensive studies of the occurrence of acidic PAH metabolites in water samples, and in soil and sediment samples after a suitable extraction step.