Validation of a gas chromatography/triple quadrupole mass spectrometry based method for the quantification of pesticides in food commodities
Article first published online: 22 DEC 2005
Copyright © 2005 John Wiley & Sons, Ltd.
Rapid Communications in Mass Spectrometry
Volume 20, Issue 3, pages 365–375, 15 February 2006
How to Cite
Vidal, J. L. M., Liébanas, F. J. A., Rodríguez, M. J. G., Frenich, A. G. and Moreno, J. L. F. (2006), Validation of a gas chromatography/triple quadrupole mass spectrometry based method for the quantification of pesticides in food commodities. Rapid Commun. Mass Spectrom., 20: 365–375. doi: 10.1002/rcm.2315
- Issue published online: 22 DEC 2005
- Article first published online: 22 DEC 2005
- Manuscript Revised: 22 NOV 2005
- Manuscript Accepted: 22 NOV 2005
- Manuscript Received: 24 SEP 2005
- Instituto Nacional de Investigación y Tecnología Agraria y Alimentaria (INIA). Grant Number: CAL03-55
A new multiresidue method has been validated in cucumber matrix for the routine analysis of 130 multiclass pesticide residues by gas chromatography/triple quadrupole mass spectrometry. The pesticides were extracted with ethyl acetate. A first identification of the pesticides was based on a tandem mass spectrometric (MS/MS) screening method, which monitors a single transition for each target compound, in less than 12 min. After that, potentially non-negative samples were analyzed again by the MS/MS confirmation/quantification method, which monitors two or three MS/MS transitions for each compound, also in less than 12 min. Performance characteristics, such as trueness, precision, linear range, detection limit (LOD) and quantification limit (LOQ), for each pesticide were calculated. The average recoveries obtained ranged between 70 and 120% at three different fortification levels (25, 200 and 500 µg/kg) with precision, expressed as relative standard deviation (RSD), values lower than 15%. The calculated LOD and LOQ were typically <3.2 and 9.6 µg/kg, respectively. Such limits were much lower than the maximum residue levels (MRLs) established by European legislation. The proposed methodology was applied to the determination of pesticides in real vegetable samples from Almería (Spain). Copyright © 2005 John Wiley & Sons, Ltd.