Dispersive solid-phase extraction followed by triethylsilyl derivatization and gas chromatography mass spectrometry for perfluorocarboxylic acids determination in water samples

J Chromatogr A. 2019 Jul 19:1597:1-8. doi: 10.1016/j.chroma.2019.03.008. Epub 2019 Mar 5.

Abstract

A new, simple derivatization method for the determination of perfluorocarboxylic acids (PFCAs, C3-C12) in water is presented. The method is based on an acid-catalyzed esterification of perfluorinated carboxylic acids with triethylsilanol. During the reaction, a triethylsilyl ester is formed which can be easily analyzed by gas chromatography-mass spectrometry (GC-MS). The classic ion exchange solid phase extraction used for PFCAs (DIN 38407-42) has been significantly modified and adopted for the newly developed derivatization method. The new method offers a linear range from 8 to 10,000 ng l-1 for PFOA, with a limit of quantification ranging from 4 to 48 ng l-1 depending on the actual PFCA. Due to sample preparation simplicity, the presented method can be applied to form PFCAs esters prior to GC-MS analysis of water samples. The method was successfully applied in the analysis of effluents from two water treatment plants in Baden-Württemberg, Germany. Additionally, to confirm the laboratory evaluation, the standard solutions and samples were also measured by an external laboratory using LC-MS2.

Keywords: Derivatization; Gas chromatography–mass spectrometry; Perfluorocarboxylic acids; Trimethylsilanol.

MeSH terms

  • Carboxylic Acids / analysis*
  • Chromatography, Liquid
  • Environmental Monitoring / methods*
  • Fluorocarbons / analysis
  • Gas Chromatography-Mass Spectrometry*
  • Germany
  • Silanes / chemistry*
  • Solid Phase Extraction*
  • Tandem Mass Spectrometry / methods
  • Water / chemistry*
  • Water Pollutants, Chemical / analysis

Substances

  • Carboxylic Acids
  • Fluorocarbons
  • Silanes
  • Water Pollutants, Chemical
  • Water