Development and independent laboratory validation of a simple method for the determination of paraquat and diquat in potato, cereals and pulses

D.I.S. Kolberg, D. Mack, M. Anastassiades, M.T. Hetmanski, R.J. Fussell, T. Meijer, J.G.J. Mol

Research output: Contribution to journalArticleAcademicpeer-review

36 Citations (Scopus)

Abstract

A new sensitive, fast and robust method for the determination of paraquat and diquat residues in potatoes, cereals and pulses is presented. Different extraction conditions (solvent, time and temperature) have been evaluated using barley grain, potatoes and dry lentils containing incurred residues of diquat and paraquat. The finalised procedure involves extraction with a mixture of methanol/water/hydrochloric acid at 80 °C and analysis by liquid chromatography–tandem mass spectrometry. Diquat D4 and Paraquat D6 internal standards were added to the test portions prior to extraction. A small-scale inter-laboratory validation of the developed method for diquat and paraquat using potato and barley samples was conducted by three laboratories. The precision and accuracy of the method were determined from recovery experiments (five replicates) at 0.01 and 0.1 mg¿kg-1. The recoveries obtained (n¿=¿180) were in the range of 92–120 % with associated relative standard deviation (RSD) between 1.4–10 % for all compound/commodity/spiking concentration combinations.
Original languageEnglish
Pages (from-to)2465-2474
JournalAnalytical and Bioanalytical Chemistry
Volume404
Issue number8
DOIs
Publication statusPublished - 2012

Keywords

  • performance liquid-chromatography
  • dilution mass-spectrometry
  • electrospray-ionization
  • chlormequat residues
  • ion suppression
  • blood
  • water
  • herbicides
  • injection
  • pears

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