Title: | A novel high-temperature combustion interface for compound-specific stable isotope analysis of carbon and nitrogen via high-performance liquid chromatography/isotope ratio mass spectrometry |
Author(s): | Federherr E; Willach S; Roos N; Lange L; Molt K; Schmidt TC; |
Address: | "Research and Innovation, Elementar Analysensysteme GmbH, Donaustr. 7, 63452, Hanau, Germany. Instrumental Analytical Chemistry, University of Duisburg-Essen, Universitatsstr. 5, 45141, Essen, Germany. Application Development Support, Agilent Technologies Sales & Services GmbH und Co.KG, Lyoner Strasse 20, 60528, Frankfurt am Main, Germany" |
Journal Title: | Rapid Commun Mass Spectrom |
ISSN/ISBN: | 1097-0231 (Electronic) 0951-4198 (Linking) |
Abstract: | "RATIONALE: In aqueous samples compound-specific stable isotope analysis (CSIA) plays an important role. No direct method (without sample preparation) for stable nitrogen isotope analysis (delta(15) N SIA) of non-volatile compounds is known yet. The development of a novel HPLC/IRMS interface based on high-temperature combustion (HTC) for both delta(13) C and delta(15) N CSIA and its proof of principle are described in this study. METHODS: To hyphenate high-performance liquid chromatography (HPLC) with isotope ratio mass spectrometry (IRMS) a modified high-temperature combustion total organic carbon analyzer (HTC TOC) was used. A system to handle a continuously large amount of water (three-step drying system), favorable carrier and reaction gas mix and flow, an efficient high-temperature-based oxidation and subsequent reduction system and a collimated beam transfer system were the main requirements to achieve the necessary performance. RESULTS: The proof of principle with caffeine solutions of the system succeeded. In this initial testing, both delta(13) C and delta(15) N values of tested compounds were determined with precision and trueness of =0.5 per thousand. Further tests resulted in lower working limit values of 3.5 mugC for delta(13) C SIA and 20 mugN for delta(15) N SIA, considering an accuracy of +/-0.5 per thousand as acceptable. CONCLUSIONS: The development of a novel HPLC/IRMS interface resulted in the first system reported to be suitable for both delta(13) C and delta(15) N direct CSIA of non-volatile compounds. This highly efficient system will probably open up new possibilities in SIA-based research fields. Copyright (c) 2016 John Wiley & Sons, Ltd" |
Keywords: | "Carbon Isotopes/*analysis/chemistry Chromatography, High Pressure Liquid/*methods Equipment Design Hot Temperature Isotope Labeling Mass Spectrometry/*methods Nitrogen Isotopes/*analysis/chemistry Reproducibility of Results;" |
Notes: | "MedlineFederherr, E Willach, S Roos, N Lange, L Molt, K Schmidt, T C eng Research Support, Non-U.S. Gov't England 2016/03/13 Rapid Commun Mass Spectrom. 2016 Apr 15; 30(7):944-52. doi: 10.1002/rcm.7524" |