UNE-EN ISO/IEC 17025:2005-accredited method for the determination of pesticide residues in fruit and vegetable samples by LC-MS/MS

Abstract

A rapid, simple and sensitive multi-residue method was developed and validated for the simultaneous quantification and confirmation of 69 pesticides in fruit and vegetables using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted following the quick, easy, cheap, effective, rugged and safe method known as QuEChERS. Mass spectrometric conditions were individually optimised for each analyte in order to achieve maximum sensitivity in multiple reaction monitoring (MRM) mode. Using the developed chromatographic conditions, 69 pesticides can be separated in less than 17 min. Two selected reaction monitoring (SRM) assays were used for each pesticide to obtain simultaneous quantification and identification in one run. With this method in SRM mode, more than 150 pesticides can be analysed and quantified, but their confirmation is not possible in all cases according to the European regulations on pesticide residues. Nine common representative matrices (zucchini, melon, cucumber, watermelon, tomato, garlic, eggplant, lettuce and pepper) were selected to investigate the effect of different matrices on recovery and precision. Mean recoveries ranged from 70% to 120%, with relative standard deviations (RSDs) lower than 20% for all the pesticides. The proposed method was applied to the analysis of more than 2000 vegetable samples from the extensive greenhouse cultivation in the province of Almeria, Spain, during one year. The methodology combines the advantages of both QuEChERS and LC-MS/MS producing a very rapid, sensitive, accurate and reliable procedure that can be applied in routine analytical laboratories. The method was validated and accredited according to UNE-EN-ISO/IEC 17025:2005 international standard (accreditation number 278/LE1027).

Liquid chromatography–electrospray ionization tandem mass spectrometry and dynamic multiple reaction monitoring method for determining multiple pesticide residues in tomato

“…However, these techniques require considerable investment in instrumentation (automated), training of staff, and have some limitations in the scope of pesticides analyzed. In 2003, Anastassiades, Lehotay, Stajnbaher, and Schenck (2003) introduced a procedure for sample preparation called QuEChERS, which has been widely used for the detection of pesticides and other compounds in a variety of matrices (Andrade, Freguglia, Furlani, Torres, & Tornisielo, 2011;Camino-Sanchez et al, 2010;GilbertLopez, Garcia-Reyes, Lozano, Fernandez-Alba, & Molina-Diaz, 2010).…”

Liquid Chromatography-Mass Spectrometry in the Analysis of Pesticide Residues in Food

“…Its sample purity requirements are not stringent, and it enables a simultaneous analysis of substances that vary considerably in polarity. The popularity of the method is confirmed by the increasing number of publications dedicated to the applications of LC-MS in the determination of contaminants, including pesticides, in food (Sivaperumal et al 2015;Gómez-Pérez et al 2015;Martinez-Dominguez et al 2015;Golge and Kebak 2015;Fillatre et al 2014;Esturk et al 2014;Oshita and Jardim 2014;González-Curbelo et al 2014;Rajski et al 2013;Arienzo et al 2013;Stachniuk and Fornal 2013;Sinha et al 2012;Gilbert-Lopez et al 2012;Lozano et al 2012;Chung and Lam 2012;BoteroCoy et al 2012;Tian 2011;Pareja et al 2011;Kmellar et al 2011;Aguilera-Luiz et al 2011;Chen et al 2011;Lehotay et al 2010;Zhang et al 2010;Camino-Sanchez et al 2010;Kamel et al 2010;Brutti et al 2010). In pesticide residue analysis, similarly to the analysis of other food contaminants, there is a distinct tendency to develop fast multiresidue methods.…”

“…The non-polar octadecylsilane phase (C 18 ) (Gómez-Pérez et al 2015;Fillatre et al 2014;AguileraLuiz et al 2011;Chung and Lam 2012;Gilbert-Lopez et al 2012;Sinha et al 2012) is commonly used as the stationary phase; the medium-polar octylsilane phase is used much more rarely (C 8 ) (Lozano et al 2012;Nunez et al 2012;Kmellar et al 2011;Ferrer et al 2011). Columns with sorbent particle diameters of 3, 3.5, 4, and 5 μm are available from a range of manufacturers, the most popular being: Zorbax (Rajski et al 2013;Lozano et al 2012;Lee et al 2009a, b;Radisic et al 2009), Atlantis (Tran et al 2012;Tseng et al 2009;Romero-Gonzalez et al 2006), Luna (Camino-Sanchez et al 2010;Lehotay et al 2010), Polaris (Anagnostopoulos et al 2012), and Phenomenex (Fillatre et al 2014). Short columns with the particle diameter not larger than 2 μm, first proposed by Waters in 2004 as BEH C 18 , with the particle diameter of 1.7 μm (Swartz 2005), are gaining increasing popularity.…”

Validação de método multirresíduo para determinação de pesticidas em alimentos empregando QuEChERS E UPLC-MS/MS

“…1 Visando proteger a saúde dos consumidores agências governamentais, como a Agência Nacional de Vigilância Sanitária (ANVISA) no Brasil, 2 limitam as quantidades de pesticidas em alimentos e estabelecem limites máximos de resíduos (LMRs) para as diversas combinações de pesticidas e commodities.…”