Determination of selected non-authorized insecticides in peppers by liquid chromatography time-of-flight mass spectrometry and tandem mass spectrometry.
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 microg 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 microg kg(-1), depending on each individual technique. Finally, the proposed methods were successfully applied to the analysis of suspected pepper samples.
Mezcua
Milagros
M
Pesticide Residue Research Group, Department of Hydrogeology and Analytical Chemistry, University of Almería, 04120 La Cañada de San Urbano, Almería, Spain.
Ferrer
Carmen
C
García-Reyes
Juan F
JF
Martínez-Bueno
María Jesús
MJ
Albarracín
Micaela
M
Claret
María
M
Fernández-Alba
Amadeo R
AR
D002138:Calibration; D002853:Chromatography, Liquid; D007202:Indicators and Reagents; D007306:Insecticides / Q000032:analysis*; D008294:Malathion / Q000032:analysis; D000073943:Neonicotinoids; D009946:Organothiophosphorus Compounds / Q000032:analysis; D029222:Piper nigrum / Q000737:chemistry*; D011725:Pyridines / Q000032:analysis; D013030:Spain; D053719:Tandem Mass Spectrometry
D007202:Indicators and Reagents; D007306:Insecticides; D000073943:Neonicotinoids; D009946:Organothiophosphorus Compounds; D011725:Pyridines; C056490:methyl isofenphos; C464843:nitenpyram; D008294:Malathion