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A multi-residue method for pesticide residue analysis in rice grains using matrix solid-phase dispersion extraction and high-performance liquid chromatography–diode array detection

Analytical and Bioanalytical Chemistry volume 397, pages 2181–2190 (2010)Cite this article

Abstract

Pesticides are widely used in rice cultivation, often resulting in detection of their residues in rice grains. So far, no analytical method has been available for the simultaneous determination of most rice pesticides in rice grains. This paper reports the development and validation of such a method for the determination of eight rice pesticides (penoxsulam tricyclazole, propanil, azoxystrobin, molinate, profoxydim, cyhalofop-butyl, deltamethrin) and 3,4-dichloroaniline, the main metabolite of propanil. Pesticide extraction and clean-up was performed by an optimized matrix solid-phase dispersion (MSPD) protocol on neutral alumina (5 g) using acetonitrile as the elution solvent. Samples were analyzed in a high-performance liquid chromatography–diode array detection (HPLC-DAD) system. Pesticide separation was achieved with a mobile phase of acetonitrile/water in a linear elution gradient from 30:70% (v/v) to 100:0% (v/v) in 14 min at a flow rate of 0.8 mL min−1. Method validation was performed by means of linearity, intra-day accuracy, inter-day precision and sensitivity. Linear regression coefficients (R 2) were always above 0.9948. Limits of detection (LOD) and quantification (LOQ) varied from 0.002 to 0.200 mg kg−1 and 0.006 to 0.600 mg kg−1, respectively. Recoveries were investigated at three fortification levels and were found to be acceptable (74–127%) with relative standard deviations (RSD) below 12%. Application of the method for the analysis of five commercial rice grain samples showed that the pesticide levels were below the LOD. Overall, the method developed is suitable for the determination of residues of most rice pesticides in rice grains at levels below the established MRLs.

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Affiliations

  1. Analytical Chemistry Laboratory, Department of Chemical Engineering, Aristotle University of Thessaloniki, 54124, Thessaloniki, Greece

    Emmanouil D. Tsochatzis & Roxani Tzimou-Tsitouridou

  2. Laboratory of Pesticide Science, Faculty of Agriculture, Aristotle University of Thessaloniki, 54124, Thessaloniki, Greece

    Urania Menkissoglu-Spiroudi

  3. Department of Biochemistry-Biotechnology, University of Thessaly, Ploutonos 26 & Aiolou Str, Larissa, 41221, Greece

    Dimitrios G. Karpouzas

Authors
  1. Emmanouil D. Tsochatzis
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  2. Urania Menkissoglu-Spiroudi
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  3. Dimitrios G. Karpouzas
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  4. Roxani Tzimou-Tsitouridou
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Correspondence to Roxani Tzimou-Tsitouridou.

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Tsochatzis, E.D., Menkissoglu-Spiroudi, U., Karpouzas, D.G. et al. A multi-residue method for pesticide residue analysis in rice grains using matrix solid-phase dispersion extraction and high-performance liquid chromatography–diode array detection. Anal Bioanal Chem 397, 2181–2190 (2010). https://doi.org/10.1007/s00216-010-3645-4

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  • DOI: https://doi.org/10.1007/s00216-010-3645-4

Keywords

  • Rice pesticides
  • Rice grains
  • HPLC
  • Matrix solid-phase dispersion (MSPD)