Skip to Content
Merck
  • Selective removal of phosphate for analysis of organic acids in complex samples.

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

Journal of chromatography. A (2015-03-01)
Sandeep Deshmukh, Andrej Frolov, Andrea Marcillo, Claudia Birkemeyer
ABSTRACT

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.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Potassium chloride, anhydrous, free-flowing, Redi-Dri, ReagentPlus®, ≥99%
Sigma-Aldrich
Potassium chloride, puriss. p.a., ≥99.5% (AT)
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, Absolute - Acetone free
Sigma-Aldrich
Potassium chloride, ReagentPlus®, ≥99.0%
Sigma-Aldrich
Potassium chloride, ACS reagent, 99.0-100.5%
Sigma-Aldrich
Methanol, suitable for HPLC, ≥99.9%
Sigma-Aldrich
Methanol, NMR reference standard
Sigma-Aldrich
Sodium phosphate dibasic solution, BioUltra, 0.5 M in H2O
Supelco
D-Mannitol, ≥99.9999% (metals basis), for boron determination
Supelco
N-Methyl-bis(trifluoroacetamide), for GC derivatization, LiChropur, ≥97.0% (GC)
Supelco
N-Methyl-bis(trifluoroacetamide), for GC derivatization, LiChropur, ≥99.0% (GC)
Sigma-Aldrich
Methoxyamine hydrochloride, 98%
Sigma-Aldrich
Potassium chloride, 99.999% trace metals basis
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Sigma-Aldrich
D-(−)-Ribose, 98%
Supelco
Potassium chloride solution, for Ag/AgCl electrodes, ~3 M KCl, saturated with silver chloride
Supelco
Potassium chloride solution, BioUltra, ~3 M in H2O
Sigma-Aldrich
D-Mannitol, tested according to Ph. Eur.
Supelco
ISA (ionic strength adjustment solution: 1 M KCl), 1 M KCl
Sigma-Aldrich
Potassium chloride solution, BioUltra, for molecular biology, ~1 M in H2O
Sigma-Aldrich
Potassium chloride, tested according to Ph. Eur.
Sigma-Aldrich
Potassium chloride, BioUltra, for molecular biology, ≥99.5% (AT)
Sigma-Aldrich
Adonitol, BioXtra, ≥99.0% (HPLC)
Millipore
D-(−)-Fructose, ≥99.0% (HPLC), suitable for microbiology
Sigma-Aldrich
D-(−)-Fructose, tested according to Ph. Eur.
Sigma-Aldrich
D-Gluconic acid solution, 49-53 wt. % in H2O
Sigma-Aldrich
Potassium chloride, AnhydroBeads, −10 mesh, 99.999% trace metals basis
Sigma-Aldrich
Potassium chloride, AnhydroBeads, −10 mesh, 99.99% trace metals basis
Sigma-Aldrich
D-(−)-Ribose, ≥98%