Quantitative and qualitative comparison of marine dissolved organic nitrogen recovery using solid phase extraction

AbstractMarine dissolved organic carbon and nitrogen (DOC and DON) are major global carbon and nutrient reservoirs, and their characterization relies on extraction methods for preconcentration and salt removal. Existing methods optimize for capturing and describing DOC. Here, we report an optimized analytical strategy to recover marine DON for subsequent molecular characterization. Retention efficiencies between 5% and 95% are reported for seven solid phase extraction (SPE) sorbents, with PPL recovering 23% of marine DON compared to 95% recovered with C18. Additional comparisons of the effect of varying sample volumes and elution speed, and the resulting molecular composition of DON extracts, were investigated using C18 and PPL sorbents. Sample volumes >200mL decreased DON retention efficiency independent of SPE sorbent, and gravity elution recovered 1.7 to 4.2fold more DON compared to vacuum elution. Characterization of extracted DON by negativeion electrospray ionization Fourier transformion cyclotron resonance mass spectrometry (FTICR MS) highlights compositional differences between DON species recovered by each method. DON isolated with optimized methods includes low molecular weight (<600Da) peptidelike compounds with low O:C ratios (0.2to0.5) that are not detected by other SPE sorbents (e.g., PPL). The majority of additional DON isolated with this approach was undetectable by direct infusion negative mode FTICR MS analysis.

Quantitative and qualitative comparison of marine dissolved organic nitrogen recovery using solid phase extraction Academic Article