Residual Analysis of Insecticides (Lambda-cyhalothrin, Lufenuron, Thiamethoxam and Clothianidin) in Pomegranate Using GC-μECD or HPLC-UVD

  • Hem, Lina (Natural Products Chemistry Laboratory, Division of Applied Bioscience and Biotechnology, College of Agriculture and Life Science, Chonnam National University) ;
  • Park, Jong-Hyouk (Natural Products Chemistry Laboratory, Division of Applied Bioscience and Biotechnology, College of Agriculture and Life Science, Chonnam National University) ;
  • Shim, Jae-Han (Natural Products Chemistry Laboratory, Division of Applied Bioscience and Biotechnology, College of Agriculture and Life Science, Chonnam National University)
  • Received : 2010.09.15
  • Accepted : 2010.09.25
  • Published : 2010.09.30


In this study, the residual levels of four insecticidal compounds (lambda-cyhalothrin, lufenuron, thiamethoxam, and clothianidin) were monitored in the pomegranate, in order to assess the risk to consumers posed by the presence of such residues. The insecticides were applied at the recommended dose rates onto pomegranate trees. The samples were then collected at harvesting time after several treatments (two, three, and four treatments). After sample preparation progressed through the clean-up procedure, lufenuron, thiamethoxam, and clothianidin residues were analyzed via a HPCL-UVD, and the lambda-cyhalothrin residue was analyzed via a GC-${\mu}ECD$. The versatility of this method was evidenced by its excellent linearity (>0.9998 to 1) at broad concentration ranges. The mean recoveries evaluated from the untreated sample spiked with two different fortification levels ranged from 72.45 to 113.90%, and the repeatability (as a relative standard deviation) resulted from triplicate recovery tests was in a range from 0.80 to 11.75%. The residues of all insecticides determined from treated pomegranate samples and their LOD levels (lunfenuron, 0.01; lambda-cyhalothrin, 0.005; thiamethoxam, 0.01; clothianidin, 0.02 mg/kg) were much lower than their MRLs (0.5 mg/kg).


  1. Ahrie, K.C., Arora, M.S., Mukherjee, S.N., 2008. Development and application of a method for analysis of lufenuron in wheat flour by gas chromatography-mass spectrometry and confirmation of bio-efficacy against Tribolium castaneum (Herbst) (Coleoptera: Tenebrionidae), J. Chromatogr. B 861, 16-21.
  2. Al-suhaibani, A.M., Ali, A.G., 2004. Susceptibility of some pomegranate fruit cultivars to myelois ceratonia zeller (Lepidoptera:phycitidae) with some notes on its population fluctuation and control measures, Minia J. of Agric. Res. & Develop. 24, 335-346.
  3. Bonafos, R., Serrano, E., Auger, P., Kreiter, S., 2007. Resistance to deltamethrin, lambda-cyholathrin and chlorpyriphos-ethyl in some populations of Typhlodromus pyri Scheuten and Amblyseius andersoni (Chant) (Acari:Phytoseiidae) from vineyards in the south-west of France, J. Crop Pro. 26, 169-172.
  4. Bouldin, J.L., Farris, J.L., Moore, M.T., Smith, Jr.S., Cooper, C. M., 2006. Hydroponic uptake of atrazine and lambda-cyhalothrin in Juncus effusus and Ludwigia peploides, Chemosphere 65, 1049-1057.
  5. Brito, N.M., Navickiene, S., Polese, L., Jardim, E.F.G., Abakerli, R.B., Ribeiro, M.L., 2002. Determination of pesticide residues in coconut water by liquidliquid extraction and gas chromatography with electron-capture plus thermionic specific detection and solid-phase extraction and high-performance liquid chromatography with ultraviolet detection, J. Chromatogr. A, 957, 201-209.
  6. Campbell, S., Chen, L., Yu, J., Li, Q.X., 2005. Adsorption and analysis of the insecticide Thiamethoxam and Indoxacarb in Hawaiian Soil, J. Agric. Food Chem. 53, 5373-5376.
  7. Cavas, T., Gozukara, S.E., 2003. Evaluation of the genotoxic potential of lambda-cyhalothrin using nuclear and nucleolar biomarkers on fish cells, Mutat. Res. Genet. Toxicol. Environ. Mutagen. 534, 93-99.
  8. Garía, M.D.G., Galera, M.M., Martínez, D.B., Gallego, J.G., 2006. Determination of benzoylureas in ground water samples by fully automated on-line pre-concentration and liquid chromatography-fluorescence detection, J. Chromatogr. A, 1103, 271-277.
  9. Gonzalez, R.R., Frenich, A.G., Vidal, J.L.M., 2008. Multiresidue method for fast determination of pesticides in fruit juice by ultra performance liquid chromatography coupled to tandem mass spectrometry, Talanta 76, 211-225.
  10. Khay, S., Choi, J.-H., Abd El-Aty, A.M., Mamun, M.I.R., Park, B.-J., Goudah, A., Shin, H.C, Shim, J.H., 2008. Dissipation Baehavior of Lufenuron, Benzoylphenylurea Isecticide, in/on Chinses Cabbage Applied by Foliar Spraying Under Greenhouse Condition, Bull. Environ. Contam. Toxicol. 81, 369-372.
  11. Palou, L., Crisosto, C.H., Garner, D., 2007. Combination of postharvest antifungal chemical treatments and controlled atmosphere storage to control gray mold and improve storability of ‘Wonderful’ pomegranates, Postharvest Biol. Technol. 43, 133-142.
  12. Rancan, M., Rossi, S., Sabatini, A.G., 2006. Determination of Thiamethoxam residues in honeybees by high performance liquid chromatography with an electrochemical detector and post-column photochemical reactor, J. Chromatogr. A, 1123, 60-65.
  13. Pandey, G., Dorrian, S.J., Russell, R.J., Oakeshott, J.G., 2009. Biotransformation of the neonicotinoid insecticides imidacloprid and thiamethoxam by Pseudomonas sp. 1G, J. Biochem. Biophys. Res. Commun. 380, 710-714.
  14. SANCO, Quality control procedures for pesticides residue analysis. European Commission, Directorate General Health and Consumer Protection. Document no. SANCO/10476/2003, February 2004.
  15. Seenivasan, S., Muraleedharan, N.N., 2009. Residues of lambda-cyhalothrin in tea, Food Chem. Toxicol. 47, 502-505.
  16. Seccia, S., Fidente, P., Montesano, D., Morrica, P., 2008. Determination of neonicotinoid insecticides in bovine milk samples by solid-phase extraction clean-up and liquid chromatography with diodearray detection, J. Chromatogr. A, 1214, 115-120.
  17. Singh, S.B., Foster, G.D., Khan, S.U., 2004. Microwave-assisted extraction for the simultaneous determination of thiamethoxam, imidacloprid, and carbndazim residues in fresh and cooked vegetable sample, J. Agric. Food Chem. 52, 105-109.

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