QuEChERS-Based Methods for the Determination of Pesticide Residues in a Dill Using Gas Chromatography with Electron Capt
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QuEChERS-Based Methods for the Determination of Pesticide Residues in a Dill Using Gas Chromatography with Electron Capture and Nitrogen Phosphorus Detection Magdalena Słowik-Borowiec 1 & Stanisław Walorczyk 2
Received: 13 August 2015 / Accepted: 2 October 2015 # Springer Science+Business Media New York 2015
Abstract In this study, three QuEChERS-based methods of improving sample extract preparation through reduction of unwanted matrix background for pesticide residue analysis in dill (a chlorophyll-containing matrix) were developed and compared. These methods involved the use of (1) dispersive solid-phase extraction (dispersive-SPE), (2) dispersive-SPE combined with liquid–liquid extraction (LLE), and (3) only LLE. Samples were analyzed by gas chromatography with electron capture and nitrogen phosphorus detection (GCECD/NPD). The results indicated that cleanup with primary secondary amine (PSA) and graphitized carbon black (GCB) sorbents followed by final solvent exchange from acetonitrile to petroleum ether was the best alternative of the tested methods, resulting in the cleanest extracts. The matrix effect of dill on the most favorable method herein was not significant, and the calibration performed well, with R2 ≥0.99. The overall recoveries at three spiking levels of 0.01, 0.1, and 1.0 mg kg−1 fell in the range between 73 and 110 % (95 % on average) with relative standard deviation (RSD) values equal to or lower than 12 % (5 % on average). Uncertainty for the studied pesticides ranged from 7 to 14 % (with the
Electronic supplementary material The online version of this article (doi:10.1007/s12161-015-0333-1) contains supplementary material, which is available to authorized users. * Magdalena Słowik-Borowiec [email protected]; [email protected] Stanisław Walorczyk [email protected] 1
Institute of Plant Protection – National Research Institute, Regional Experimental Station, Gen. Langiewicza 28, 35-101 Rzeszów, Poland
2
Institute of Plant Protection – National Research Institute, WładysławaWęgorka 20, 60-318 Poznań, Poland
overall average uncertainty of 11 %). Analyses of real samples revealed the presence of pesticides unapproved for use on dill, as well as exceedances of the maximum residue levels (MRLs) for some pesticides. The samples with residue violation results were also confirmed by gas chromatography–tandem mass spectrometry (GC-MS/MS). The proposed method of sample preparation and chromatographic analysis is sufficient and can be applied with all certainty to determine pesticide residues in dill and other plants of high pigment content, i.e., chlorophyll. Keywords Pesticide residue analysis . Gas chromatography . Dispersive solid-phase extraction . Liquid–liquid extraction . Dill (Anethum graveolens L.)
Introduction Dill (Anethum graveolens L.) probably originates from the region of Southwest Asia or Southeast Europe (Bailer et al. 2001). In many countries, dill has long been cultivated as a spice plant, and due to its unique chemical composition, it also has therapeutic
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