TY - JOUR AU - Wang, Liming AU - Amelung, Wulf AU - Willbold, Sabine TI - 18 O Isotope Labeling Combined with 31 P Nuclear Magnetic Resonance Spectroscopy for Accurate Quantification of Hydrolyzable Phosphorus Species in Environmental Samples JO - Analytical chemistry VL - 93 IS - 4 SN - 1520-6882 CY - Columbus, Ohio PB - American Chemical Society M1 - FZJ-2021-03106 SP - 2018 - 2025 PY - 2021 AB - 31P nuclear magnetic resonance (NMR) spectra can be biased due to the hydrolysis of labile P species during sample treatment and NMR analysis. This paper offers an approach to circumvent this problem by performing sample preparation and analysis in 18O-enriched medium. Heavy 18O isotope atoms were introduced into the resulting artificial hydrolysis products. The NMR signal of 18O-labeled P was shifted upfield relative to the unlabeled P nuclei in natural metabolites. This isotope shift enabled an immediate differentiation of artificial hydrolysis products from natural metabolites. Moreover, the hydrolysis products could be accurately quantified. Our data suggest that the extent to which artificial hydrolysis alters NMR spectra varies among different types of environmental samples. For instance, 72–84% of the detected monoesters in the organic soils of this study were actually artificially hydrolyzed diesters. By contrast, artificial hydrolysis products in the mineral soils used for this study accounted for less than 6% of the total monoesters. Polyphosphate was also hydrolyzed to yield 18O-labeled products in algal biomass. LB - PUB:(DE-HGF)16 C6 - 33393290 UR - <Go to ISI:>//WOS:000618089100020 DO - DOI:10.1021/acs.analchem.0c03379 UR - https://juser.fz-juelich.de/record/894217 ER -