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Determination of selected non-authorized insecticides in peppers by liquid chromatography time-of-flight mass spectrometry and tandem mass spectrometry

Mezcua, M., Ferrer, C., García-Reyes, J.F., Martínez-Bueno, M.J., Albarracín, M., Claret, M., Fernández-Alba, A.R.

Rapid Communications in Mass Spectrometry 22 (9), pp. 1384-1392


In this work, two analytical methods based on liquid chromatography coupled to electrospray time-of-flight mass spectrometry (LC/ESI-TOFMS) and tandem mass spectrometry (LC/ESI-MS/MS) are described for the identification, confirmation and quantitation of three insecticides non-authorized in the European Union (nitenpyram, isocarbophos and isofenphos-methyl) but detected in recent monitoring programmes in pepper samples. The proposed methodologies involved a sample extraction procedure using liquid-liquid partition with acetonitrile followed by a cleanup step based on dispersive solid-phase extraction. Recovery studies performed on peppers spiked at different fortification levels (10 and 50 μg kg-1) yielded average recoveries in the range 76-100% with relative standard deviation (RSD) (%) values below 10%. Identification, confirmation and quantitation were carried out by LC/TOFMS and LC/MS/MS using a hybrid triple quadrupole linear ion trap (QqLIT) instrument in multiple-reaction monitoring (MRM) mode. The obtained limits of quantitation (LOQs) were in the range 0.1-5 μg kg-1, depending on each individual technique. Finally, the proposed methods were successfully applied to the analysis of suspected pepper samples.

Copyright © 2008 John Wiley & Sons, Ltd. 2008,


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Published 11-12-2008, 11:13:47


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