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Survey of low-level endocrine disrupting pesticides in food matrices in Slovakia
Authors:Svetlana Hrouzková  Eva Matisová  Mária Andra??íková  Matej Horváth  Renáta Hú?ková  Jarmila ?ur?anská
Institution:1. Institute of Analytical Chemistry, Faculty of Chemical and Food Technology, Slovak University of Technology in Bratislava , Radlinského 9 , 812 37 Bratislava , Slovak Republic svetlana.hrouzkova@stuba.sk;3. Institute of Analytical Chemistry, Faculty of Chemical and Food Technology, Slovak University of Technology in Bratislava , Radlinského 9 , 812 37 Bratislava , Slovak Republic;4. State Veterinary and Food Institute in Bratislava , Botanická 15 , 842 52 Bratislava , Slovak Republic
Abstract:The search on endocrine disrupting chemicals (EDCs) in non-fatty food was evaluated. A fast, high-throughput, accurate, multiresidue method for the analysis of selected EDC pesticides in fruit and vegetable food samples was developed. The QuEChERS technique was used for sample preparation. Fast GC-MS was performed with a narrow-bore capillary column and a quadrupole benchtop detector with electron ionization (EI) and negative chemical ionization (NCI). A part of the work was devoted to the comparison of NCI versus EI approach concerning the sensitivity of detection and to the study of selectivity enhancement in NCI mode. Matrix-matched standard solutions were utilized for calibration. The methods validation was performed. Fortification studies at 1, 5, 10 and 250?µg?kg?1 for 35 pesticides in EI mode and 0.1, 1, 5 and 250?µg?kg?1 for 28 pesticides in NCI mode were performed. Average recoveries for each fortification level ranged from 70 to 110% with >80% of recoveries between 90 and 110%. Limits of quantification (LOQs) were established at 5?µg?kg?1 for EI and at 1?µg?kg?1 for NCI mode, which is lower than the lowest maximum residue level (MRL) value set by the European Commission in fruit and vegetables. The developed and validated fast GC-MS method was successfully applied to the search of EDC pesticides at ultratrace concentration level in real fruit and vegetable samples in Slovakia. Thirty-four samples of 20 different commodities were analyzed. Seven samples contained residues of three or more EDCs pesticides.
Keywords:endocrine disrupting chemicals  pesticides  fast GC  electron ionization  negative chemical ionization  non-fatty food samples  ultratrace analysis
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