Abstract
Trace level analyses in complex matrices benefit from heart-cut multidimensional gas chromatographic (MDGC) separations and quantification via a stable isotope dilution assay. Minimization of the potential transfer of co-eluting matrix compounds from the first dimension (1D) separation into the second dimension separation requests narrow cut-windows. Knowledge about the nature of the isotope effect in the separation of labeled and unlabeled compounds allows choosing conditions resulting in at best a co-elution situation in the 1D separation. Since the isotope effect strongly depends on the interactions of the analytes with the stationary phase, an appropriate separation column polarity is mandatory for an isotopic co-elution. With 3-alkyl-2-methoxypyrazines and an ionic liquid stationary phase as an example, optimization of the MDGC method is demonstrated and critical aspects of narrow cut-window definition are discussed.
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Acknowledgments
The authors are particularly grateful to Supelco (Sigma-Aldrich; SILEP program) for the ionic liquid separation columns evaluated in this work. C. Legrum is grateful to the “Graduiertenförderung des Landes Rheinland-Pfalz” for a Ph.D. scholarship. Also, financial support from the Ministerium für Umwelt, Landwirtschaft, Ernährung, Weinbau und Forsten (Rheinland-Pfalz, Germany) is gratefully acknowledged.
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Hans-Georg Schmarr and Charlotte Legrum contributed equally to this work.
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Schmarr, HG., Slabizki, P. & Legrum, C. Optimization in multidimensional gas chromatography applying quantitative analysis via a stable isotope dilution assay. Anal Bioanal Chem 405, 6589–6593 (2013). https://doi.org/10.1007/s00216-013-7072-1
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DOI: https://doi.org/10.1007/s00216-013-7072-1