TWO-DIMENSIONAL ION CHROMATOGRAPHY TANDEM-MASS SPECTROMETRIC (2D-IC-MS/MS) METHOD FOR THE ANALYSIS OF PHOSPHORUS COMPOUNDS IN SOIL

Abstract

Investigations into soil organic phosphorus (Po) dynamics are instrumental in understanding the transformations and processes responsible for ecosystem productivity. However, quantitative analysis of Po in a soil environment is extremely challenging due to low target analyte concentrations and matrix interferences with chromatography and analysis. Consequently, a two-dimensional ion chromatography-tandem mass spectrometric (2D-IC-MS/MS) method was developed to estimate soil Po concentrations. The first dimension diverted early eluting anions to waste while preconcentrating P compounds in a trap column, followed by chromatographic separation and detection in the second dimension. Detection was done using a mass spectrometer, and quantification was performed using the multiple reaction monitoring scan (MRM) method. The linear range of the studied P compounds, mostly nucleotides, was 0.05 – 50 ng/mL. Most P compounds were detected and quantified in calcareous subsoil samples in the concentration ranges 0.70 – 51.78 ng/g. The developed method achieved chromatographic separation that allowed unambiguous identification of isobars/isomers and isotopologues contributing to interferences in MS detection. However, improvements to the extraction method and post-clean-up procedures are required due to the complexity of soil extract composition, extreme matrix effect and/or loss of analyte during preconcentration. The method is ideal for simultaneously analyzing P compounds from environmental samples to elucidate key components of the soil P dynamics.