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  • 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: Federherr E, Willach S, Roos N, Lange L, Molt K, Schmidt TC.
    Journal: Rapid Commun Mass Spectrom; 2016 Apr 15; 30(7):944-52. PubMed ID: 26969937.
    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 (δ(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 δ(13) C and δ(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 δ(13) C and δ(15) N values of tested compounds were determined with precision and trueness of ≤0.5 ‰. Further tests resulted in lower working limit values of 3.5 μgC for δ(13) C SIA and 20 μgN for δ(15) N SIA, considering an accuracy of ±0.5 ‰ as acceptable. CONCLUSIONS: The development of a novel HPLC/IRMS interface resulted in the first system reported to be suitable for both δ(13) C and δ(15) N direct CSIA of non-volatile compounds. This highly efficient system will probably open up new possibilities in SIA-based research fields. Copyright © 2016 John Wiley & Sons, Ltd.
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