Trace determination of sulfonylurea herbicides in water and grape samples by capillary zone electrophoresis using large volume sample stacking

Department of Analytical Chemistry, University of Granada, Campus Fuentenueva, s/n, 18071 Granada, Spain.
Analytical and Bioanalytical Chemistry (Impact Factor: 3.44). 05/2010; 397(6):2593-601. DOI: 10.1007/s00216-010-3812-7
Source: PubMed


A sensitive and reliable method using capillary zone electrophoresis with UV-diode array detection has been developed and validated for trace determination of residues of sulfonylurea herbicides in environmental water samples and grapes from different origins. The analytes included are triasulfuron, rimsulfuron, flazasulfuron, metsulfuron-methyl, and chlorsulfuron. Optimum separation has been achieved on a 48.5-cm x 50-microm (effective length 40 cm) bubble cell capillary using 90 mM ammonium acetate buffer, pH 4.8, by applying a voltage of 20 kV at 25 degrees C and using p-aminobenzoic acid as the internal standard. In order to increase sensitivity, large volume sample stacking with polarity switching has been applied as on-line preconcentration methodology. For water samples, a solid-phase extraction (SPE) procedure based on the use of Oasis HLB cartridges was applied for off-line preconcentration and cleanup. For grape samples, the SPE procedure was achieved with C(18) sorbent, after extraction of the compounds with MeOH:H(2)O (1:1) by sonication. The limits of detection for the studied compounds were between 0.04 and 0.12 microg/L for water samples and 0.97 and 8.30 microg/kg in the case of grape samples, lower in all cases than the maximum residue limits permitted by the EU for this kind of food. The developed methodology has demonstrated its suitability for the monitoring of these residues in environmental water and grape samples with high sensitivity, precision, and satisfactory recoveries.

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Available from: Ana M. García-Campaña, Apr 23, 2014
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    • "Several analytical methods have been reported for trace level determination of SUHs in various matrices (Berrada et al. 2003), including enzyme-linked immunosorbent assay (Degelmann et al. 2004), high-performance liquid chromatography (HPLC) with various detectors, such as diode array detector (DAD) (Zhou et al. 2006; Niu et al. 2009; Gallitzendörfer et al. 2011; Tsochatzis et al. 2012), mass spectrometry (MS) (Rodríguez and Orescan 1998; Ayano et al. 2004; Ouyang et al. 2009), and tandem mass spectrometry (MS/MS) (Baker et al. 2005; Fang et al. 2010; Yan et al. 2011; Kang et al. 2011; Fenoll et al. 2012), capillary highperformance liquid chromatography (capillary HPLC) with DAD (Bouri et al. 2012; Lerma-García et al. 2013; Gure et al. 2013), micellar electrokinetic capillary chromatography (MEKC) with DAD (Dinelli et al. 1995; Penmetsa et al. 1997), and capillary electrophoresis with DAD (Berger and Wolfe 1996; Hickes and Watrous 1999; Chen et al. 2000; Quesada-Molina et al. 2010). On the other hand, due to their occurrence levels and complexity of the food matrices, determination of SUH residues requires sample preparation before their final determinations . "
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    ABSTRACT: In this study a simple, rapid, and efficient method has been developed for the determination of six sulfonylurea herbicides (SUHs): triasulfuron, metsulfuron-methyl, chlorsulfuron, flazasulfuron, chlorimuron-ethyl, and primisulfuron-methyl in commercial grape and apple juice samples, using dispersive liquid–liquid microextraction coupled with capillary high-performance liquid chromatography with diode array detection. Various parameters that influence the extraction efficiency, such as the type and volume of extraction and disperser solvents, sample pH, and salt addition, were investigated and optimized. Under the optimum conditions, limits of detection and quantification of the method were in the ranges of 2–9 and 8–29 μg L−1, respectively, lower than the maximum residue limits set by the European Union for the raw fruits, such as grape and apple. The intra- and inter-day relative standard deviations varied from 1.0 to 8.2 and 1.8 to 9.8 %, respectively, with recoveries between 72.0 and 109.5 % for commercial grape (both white and red) and apple juice samples, showing satisfactory accuracy for the determination of SUHs in fruit juices.
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