Direkt zum Inhalt
Merck

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
ZUSAMMENFASSUNG

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.

MATERIALIEN
Produktnummer
Marke
Produktbeschreibung

Sigma-Aldrich
Methanol, suitable for HPLC, ≥99.9%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Kaliumchlorid, ACS reagent, 99.0-100.5%
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, ≥99.9%
Sigma-Aldrich
Natriumphosphat, ACS reagent, ≥99.0%
Sigma-Aldrich
Ameisensäure, reagent grade, ≥95%
Sigma-Aldrich
Pyridin, ACS reagent, ≥99.0%
Sigma-Aldrich
Methanol, HPLC Plus, ≥99.9%
Sigma-Aldrich
Ameisensäure, ACS reagent, ≥96%
Sigma-Aldrich
Ameisensäure, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥98%
Sigma-Aldrich
D-(−)-Fructose, ≥99% (HPLC)
Sigma-Aldrich
Natriumfluorid, ACS reagent, ≥99%
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Sigma-Aldrich
Kaliumchlorid, for molecular biology, ≥99.0%
Sigma-Aldrich
Natriumphosphat, puriss. p.a., ACS reagent, anhydrous, ≥99.0% (T)
Sigma-Aldrich
Pyridin, suitable for HPLC, ≥99.9%
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, suitable as ACS-grade LC reagent, ≥99.9%
Sigma-Aldrich
Kaliumchlorid, puriss., meets analytical specification of Ph. Eur., BP, USP, FCC, E508, 99-100.5% (AT), ≤0.0001% Al