Measurement of δ13C values of soil amino acids by GC–C–IRMS using trimethylsilylation: a critical assessment

Abstract

In this study, we evaluated trimethylsilyl (TMS) derivatives as derivatization reagents for the compound-specific stable carbon isotope analysis of soil amino acids by gas chromatography–combustion–isotope ratio mass spectrometry (GC–C–IRMS). We used non-proteinogenic amino acids to show that the extraction–derivatization–analysis procedure provides a reliable method to measure δ13C values of amino acids extracted from soil. However, we found a number of drawbacks that significantly increase the final total uncertainty. These include the following:production of multiple peaks for each amino acid, identified as di-, tri- and tetra-TMS derivatives;a number of TMS-carbon (TMS-C) atoms added lower than the stoichiometric one, possibly due to incomplete combustion;different TMS-C δ13C for di-, tri- and tetra-TMS derivatives.For soil samples, only four amino acids (leucine, valine, threonine and serine) provide reliable δ13C values with a total average uncertainty of 1.3 ‰. We conclude that trimethylsilyl derivatives are only suitable for determining the 13C incorporation in amino acids within experiments using 13C-labelled tracers but cannot be applied for amino acids with natural carbon isotope abundance until the drawbacks described here are overcome and the measured total uncertainty significantly decreased.