Comprehensive Method Validation for the Determination of 170 Pesticide Residues in Pear Employing Modified QuEChERS With
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Comprehensive Method Validation for the Determination of 170 Pesticide Residues in Pear Employing Modified QuEChERS Without Clean-Up and Ultra-High Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry Magali Kemmerich 1 & Gabrieli Bernardi 1 & Osmar D. Prestes 1 & Martha B. Adaime 1 & Renato Zanella 1
Received: 15 May 2017 / Accepted: 20 August 2017 # Springer Science+Business Media, LLC 2017
Abstract A fast ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) method was developed for quantitative determination of pesticide residues in pear. A fast modified acetate QuEChERS method without clean-up was used for sample preparation. Validation was performed according to SANTE guideline. Matrix effect results were significative for most part of compounds and thus a matrix-matched calibration was employed. The linear range of the method was from 2.5 to 100 μg kg−1. Recoveries were between 70 and 120% with precision ≤ 20%. Limit of quantification was 2.5 μg kg−1 for most compounds. Uncertainty results ranged from 22 to 49%. In real sample analyses, 21 compounds were quantified in concentrations between 3.3 and 1427 μg kg−1. Method proved to be simple, robust and effective to be applied in routine analysis. Keywords Pesticide residues . Pear . Validation criteria . QuEChERS . UHPLC-MS/MS
Introduction Inappropriate agricultural practice for the use of pesticides incur in residues occurrence that, at levels above the maximum residue limits (MRL), might be a risk to human health (Gibney et al. 2009). According to Food and Agriculture
* Renato Zanella [email protected] 1
Laboratory of Pesticide Residues Analysis (LARP), Chemistry Department, Federal University of Santa Maria, Santa Maria, RS 97105-900, Brazil
Organization (FAO), Bresidue^ is the fraction of a substance, its metabolites, conversion or reaction products, and impurities that remain in food from agricultural products and/or animals treated with these substances (FAO 2011). Each country has established the MRL for pesticide residues in food matrices (Global MRLs 2015) and maintain monitoring programs, in different extensions, to ensure food safety. To monitor pesticides occurrence in cultures, the optimal extraction procedure is the one that allows the determination of a higher number of compounds, called a multiresidue method. The sample preparation step and the operations involved can affect the result and thus need a suitable procedure to obtain the right information in the analysis (Fenik et al. 2011). Miniaturized methods such as solid-phase microextraction (SPME) (Xu et al. 2016), stirring bar sorptive extraction (SBSE) (Kawaguchi et al. 2013), and others like pressurized liquid extraction (PLE) (Vazquez-Roig and Picó 2015), microwave-assisted extraction (MAE) (Wang et al. 2016), matrix solid-phase dispersive (MSPD) (Carro et al. 2017), and ultrasonic extraction (USE) (Pan et al. 2008) have proven to be fast and efficient techniques for many types of food samples. However, the different ph
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