Premium
Determination of selected non‐authorized insecticides in peppers by liquid chromatography time‐of‐flight mass spectrometry and tandem mass spectrometry
Author(s) -
Mezcua Milagros,
Ferrer Carmen,
GarcíaReyes Juan F.,
MartínezBueno María Jesús,
Albarracín Micaela,
Claret María,
FernándezAlba Amadeo R.
Publication year - 2008
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.3515
Subject(s) - chemistry , chromatography , mass spectrometry , selected reaction monitoring , electrospray , liquid chromatography–mass spectrometry , tandem mass spectrometry , electrospray ionization , sample preparation , solid phase extraction , detection limit , analytical chemistry (journal)
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.