Journal
MICROCHIMICA ACTA
Volume 182, Issue 1-2, Pages 95-103Publisher
SPRINGER WIEN
DOI: 10.1007/s00604-014-1290-x
Keywords
Pesticides; Solid-phase extraction; Multiwalled carbon nanotubes; Liquid-chromatography-mass spectrometry
Categories
Funding
- Agencia Espanola de Cooperacion Internacional (AECI) [Accion Integrada A1/035959/11]
- Agencia Espanola de Cooperacion Internacional [A1/035959/2011]
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We describe a MWCNT-based method for the solid-phase extraction of eight pesticides from environmental water samples. The analytes are extracted from 100 mL samples at pH 5.0 (containing 5 mmol L-1 of KCl) by passing the solution through a column filled with 20 mg of multiwalled carbon nanotubes. Following elution, the pesticides were determined by LC and electrospray ionization hybrid quadrupole linear ion trap MS. Two selected reaction monitoring transitions were monitored per compound, the most intense one being used for quantification and the second one for confirmation. In addition, an information-dependent acquisition experiment was performed for unequivocal confirmation of positive findings. Matrix effect was not found in real waters and therefore the quantitation was carried out with calibration graphs built with solvent based standards. Except for cymoxanil, the detection and quantitation limits in surface waters are in the range from 0.3 to 9.5 ng L-1 and 1.6 to 45.2 ng L-1, respectively. Recoveries from spiked ultrapure water are similar to 100 %, except for the most polar pesticides methomyl and cymoxanil. The same behavior is found for real water samples (except for phosalone). The relative standard deviation is < 10 % in all cases.
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