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

Erik Maloschik, Mária Mörtl, A. Székács

Research output: Contribution to journalArticle

18 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 2010

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Carbamates
Herbicides
Gas chromatography
Gas Chromatography-Mass Spectrometry
Mass spectrometry
2-Methyl-4-chlorophenoxyacetic Acid
Gases
Electrons
Derivatives
2,4-Dichlorophenoxyacetic Acid
Acids
Hungary
Groundwater
Limit of Detection
Esters
Impact ionization
Mass spectrometers
Ions
Surface waters
Water

Keywords

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

ASJC Scopus subject areas

  • Analytical Chemistry
  • Biochemistry

Cite this

Novel derivatisation technique for the determination of chlorophenoxy acid type herbicides by gas chromatography-mass spectrometry. / Maloschik, Erik; Mörtl, Mária; Székács, A.

In: Analytical and Bioanalytical Chemistry, Vol. 397, No. 2, 05.2010, p. 537-548.

Research output: Contribution to journalArticle

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