Selective removal of phosphate for analysis of organic acids in complex samples

• 17 anion exchange SPE materials were screened and tested for separation of phosphate from organic acids.
• Polymer-based SPE materials generally provided a favorable selectivity for organic acid recovery.
• Greater than 98% of phosphate removal was achieved by anion exchange SPE.
• Obtained optimum recoveries were >80% for sugars and <80% for organic acids.
• Anion exchange SPE outperforms the selectivity of precipitation as traditional approach of phosphate removal.

Accurate quantitation of compounds in samples of biological origin is often hampered by matrix interferences one of which occurs in GC-MS analysis from the presence of highly abundant phosphate. Consequently, high concentrations of phosphate need to be removed before sample analysis. Within this context, we screened 17 anion exchange solid-phase extraction (SPE) materials for selective phosphate removal using different protocols to meet the challenge of simultaneous recovery of six common organic acids in aqueous samples prior to derivatization for GC-MS analysis. Up to 75% recovery was achieved for the most organic acids, only the low pKa tartaric and citric acids were badly recovered. Compared to the traditional approach of phosphate removal by precipitation, SPE had a broader compatibility with common detection methods and performed more selectively among the organic acids under investigation. Based on the results of this study, it is recommended that phosphate removal strategies during the analysis of biologically relevant small molecular weight organic acids consider the respective pKa of the anticipated analytes and the detection method of choice.