Determination of Over 350 Multiclass Pesticides in Jams by Ultra-High Performance Liquid Chromatography Time-of-Flight M
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Determination of Over 350 Multiclass Pesticides in Jams by Ultra-High Performance Liquid Chromatography Time-of-Flight Mass Spectrometry (UHPLC-TOFMS) Patricia Pérez-Ortega 1 & Felipe J. Lara-Ortega 1 & Juan F. García-Reyes 1 & Miriam Beneito-Cambra 1 & Bienvenida Gilbert-López 1 & Natividad Ramos Martos 1 & Antonio Molina-Díaz 1
Received: 4 September 2015 / Accepted: 16 November 2015 # Springer Science+Business Media New York 2015
Abstract In this study, a screening method was developed using ultra-high performance liquid chromatography time-of-flight mass spectrometry (UHPLC-TOFMS) for multiclass pesticide analysis in jam samples. The method was based on an experimental database with retention time/accurate mass data for the 353 selected analytes. Compound identification was based on retention time and the accurate mass measurements of the protonated molecules. The limits of detection were below 10 μg kg−1 for 90 % of the studied compounds. The proposed method was successfully applied to evaluate the presence and concentration levels of over 350 multiclass pesticides in a total of 54 jam market samples collected in Spain from different companies. Results found were in compliance with the current regulations with the exception of a sample, which contained monocrotophos. Forty-one percent of the samples were found free of pesticides; 26 % of the samples contained only one pesticide while 33 % contained at least two or more pesticides.
Keywords Pesticides . Food . Jams . Liquid chromatography . Mass spectrometry Electronic supplementary material The online version of this article (doi:10.1007/s12161-015-0369-2) contains supplementary material, which is available to authorized users. * Antonio Molina-Díaz [email protected] 1
Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaén, 23071 Jaén, Spain
Introduction Over 1000 active substances against pests are used worldwide in current agricultural practice due to its undisputable benefits for crop protection (Tomlin 2011). Their application results in improved crop yields and enables international trade and consumption of fresh fruits and vegetables. However, some pesticides may eventually cause a range of adverse effects on human health. Thus, different organizations have established regulatory controls intended to limit exposure of the general population to pesticide residues (European Union (EU) 2000) by setting maximum residue levels (MRLs) for selected pesticide/commodity combinations usually in the range 0.01–10 mg kg−1 (European Union (EU) 2005, 2006, 2008a, b). These low MRLs and the great number of potential residues have prompted the development and improvement of multi-residue methods (MRMs), which should be comprehensive in order to enable official laboratories to exert an effective control (Fernández-Alba 2004; Fernández-Alba and GarcíaReyes 2008). Up-to-date liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) using triple quadrupole instrumentation operated in the selected reaction monit
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