VALIDATION OF A METHODOLOGY FOR DETECTING 247 PESTICIDES IN LOW WATER CONTENTS FOOD MATRICES BY LC-MS/MS AND GC-MS/MS

ALVA, MARIANA; KAMIYA, NORMA; LACINA, MARINA; BRITO, JAVIER; NAVARRO, MARÍA E.; SOROL, PABLO

Foz do Iguazu

Workshop; 7º Latin American Pesticide Residue Workshop; 2019

UFSM

VALIDATION OF A METHODOLOGY FOR DETECTING 247 PESTICIDES IN LOW WATER CONTENTS FOOD MATRICES BY LC-MS/MS AND GC-MS/MSMarina Lacina1, María E. Navarro1, Mariana Alva1, Javier Brito1, Pablo Sorol1, Anahí Charaf1, Norma Kamiya11Laboratorio de Residuos de Plaguicidas (LRP), Estación Experimental Obispo Colombres (EEAOC), Av. W. Cross 3150, Las Talitas, CP 4101, Tucumán, Argentina E-mail: plaguicidas@eeaoc.org.arThe main objective of this work was to optimize a gas and liquid chromatography coupled to tandem triple quadrupole mass spectrometry (GC-MS/MS and LC-MS/MS) methodology that would enable our laboratory to analyze pesticides residue in low content water food matrices. The validated methodology covered the detection of 247 pesticides, including insecticides, herbicides, acaricides and fungicides, in wheat, wheat flour, dehydrated lemon peel and chia.The QuEChERS EN 15662:2008 method [1], with magnesium sulfate and buffer citrate in sample preparation was used. In order to quantify and confirm pesticides analyzed by liquid chromatography, a Shimadzu Nexera liquid chromatograph with a ABSciex triple quadrupole 5500 detector was used, under chromatographic and instrumental conditions described in the IMethod Application for Cliquid Software ABSciex [2]. In order to analyze pesticides by GC, an Agilent Technologies 7890A GC System coupled to a triple Quad 7000 detector was used.Validation was carried out as indicated in SANTE/11813/2017 [3]. Intermediate precision, trueness (expressed as recovery %), matrix effect, Limit of Detection (LOD), Limit of Quantitation/Report Limit (LOQ/RL), linearity, working range and uncertainty were evaluated.The average validation data of the method are shown in Table No. 1Table Nº1ParameterResultAcceptance CriteriaLOD (mg/kg)0.010-0.025---LOQ/RL (mg/kg)0.020-0.050≤ MRLIntermediate precision (SRD)9 ≤ 20Trueness as mean recovery (%) 99 (LC) 109 (GC)70-120%Linearity (R2)≥ 0.99≥ 0.99Working range (mg/kg)0.010-1 (LC)0.010-2.0 (GC)--Expanded uncertainty32% (LC)29 % (GC)