Novel derivatisation technique for the determination of chlorophenoxy acid type herbicides by gas chromatography-mass spectrometry

Erik Maloschik, Mária Mörtl, András Székács

Research output: Contribution to journalArticle

19 Citations (Scopus)

Abstract

The analytical detection of chlorophenoxycarboxylic-acid-type herbicides (2,4-D, dichloprop, MCPA, etc.) in environmental samples is often a problem in instrumental analysis, as these compounds containing free carboxylic groups require chemical derivatisation prior to gas chromatographic (GC) methods. Nine chlorophenoxy-acid-type herbicide active ingredients have been derivatised successfully with trimethylsilyl N,N-dimethyl carbamate and t-butyldimethylsilyl N,N-dimethyl carbamate by forming their trimethylsilyl (TMS) and t-butyldimethylsilyl (TBDMS) esters, respectively. The detection and determination of the derivatives were performed by capillary gas chromatography-mass spectrometry. The study included determination of retention indices, mass spectral properties and comparison of derivatives produced. The mass spectra of TBDMS derivatives are usually dominated by very characteristic ions [M-57]+ resulting from the cleavage of t-butyl moiety during electron impact (EI) ionisation in the mass spectrometer. Limits of detection were 5 to 100 pg applying GC with EI-MS detection in full scan mode. The method, using SPE sample preparation, was applied for the analysis of 115 ground water and surface water samples collected in Békés County, Hungary in 2009.

Original languageEnglish
Pages (from-to)537-548
Number of pages12
JournalAnalytical and Bioanalytical Chemistry
Volume397
Issue number2
DOIs
Publication statusPublished - May 1 2010

Keywords

  • Chlorophenoxy acids
  • Derivatisation
  • Gas chromatography
  • Mass spectrometry
  • Residue analysis
  • Silyl carbamates
  • Silylation

ASJC Scopus subject areas

  • Analytical Chemistry
  • Biochemistry

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