COMBINING QuEChERS PREPARATION AND MICELLAR ELECTROKINETIC CHROMATOGRAPHY FOR DETERMINATION OF NEONICOTINOID INSECTICIDES IN FRUITS AND VEGETABLES

D. S. Bol’shakov, V. G. Amelin, T. B. Nikeshina

Аннотация


The possibility of electrophoretic separation and simultaneous determination of 7 neonicotinoids (imidacloprid, acetamiprid, thiamethoxam, thiacloprid, nitenpyram, clothianidin and dinotefuran) by micellar electrokinetic chromatography is shown. We propose a method for extracting and concentrating of neonicotinoid insecticides from vegetables and fruits using the sample preparation QuEChERS. The optimum compositions of the salting-out mixtures for extraction and sorbents for purification of the resulting extracts from vegetables and fruits were selected. Extraction of pesticides from the fruits was performed by acetonitrile using a mixture of sodium citrates (Na3C6H5O7·2H2O, Na2HC6H5O7·1,5Н2О) with the following clean-up of 2 ml of the extract with sorbent PSA (100 mg) and anhydrous magnesium sulfate (300 mg). During the analysis of vegetables ethyl acetat was used as an extractant in the presence of anhydrous magnesium sulfate and sodium chloride with the following clean-up of 2 ml of the extract with sorbent PSA (100 mg) and graphitized carbon black (10 mg). In optimal conditions the recovery of the analytes ranged from 62 to 81 % for fruits and from 38 to 76 % for vegetables. The limits of quantification of neonicotinoids with a 10.0 g weight sample were from 0.25 to 0.65 mg·kg-1 and from 0.04 to 0.13 mg·kg-1 for fruits and vegetables respectively. The relative standard deviation of the test results does not exceed 0.1. Duration of analysis is 1-1.5 hr.

Key words: neonicotinoids, micellar electrokinetic chromatography, QuEChERS, vegetables, fruits

(Russian)

DOI:http://dx.doi.org/10.15826/analitika.2015.19.1.003

 

D.S. Bol’shakov1, V.G. Amelin1,2, T.B. Nikeshina1

 1Federal Centre for Animals Health (ARRIAH), Yur’evets, Vladimir, Russian Federation

2Vladimir State University named after Alexander and Nikolay Stoletovs, Vladimir, Russian Federation


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Литература


Watanabe E., Baba K., Eun H., Miyake S. Application of a commercial immunoassay to the direct determination of insecticide imidacloprid in fruit juices. Food Chem., 2007, vol. 102, pp. 745-750. doi: 10.1016/j.foodchem.2006.06.031.

Xu T., Wei K.Y., Wang J., Ma H.X., Li J. Quantitative analysis of the neonicotinoid insecticides imidacloprid and thiamethoxam in fruit juices by enzyme-linked immunosorbent assays. J. AOAC Int., 2010, vol. 93, no. 1, pp. 12-18.

Liu S., Wei Z.Z.F., Ren Y., Gui W., Wu H., Zhu G. Simultaneous determination of seven neonicotinoid pesticide residues in food by ultra-performance liquid chromatography tandem mass spectrometry. J. Agric. Food. Chem., 2010, vol. 58, pp. 3271-3278. doi: 10.1021/jf904045j.

Chin-Chen M.L., Esteve-Romero J., Carda-Broch S. Determination of the insecticide imidacloprid in fruit juices usingmicellar high-performance liquid chromatography. J. AOAC Int., 2009, vol. 92, no 5. pp, 1551-1556.

Vedishcheva D.V., Soboleva I.G. [Study of the conditions for trace quantities of neonicotinoid insecticide residues by high performance liquid chromatography]. Sorbts. i khromatogr. protsessy [Sorpt. and chromatogr. processes], 2009, vol. 9, no. 1, pp. 154-163 (in Russian).

Watanabe E., Baba K., Eun H. Simultaneous determination of neonicotinoid insecticides in agricultural samples by solid-phase extraction cleanup and liquid chromatography equipped with diode-array detection. J. Agric. Food. Chem., 2007, vol. 55, pp. 3798-3804. doi: 10.1021/jf063140m.

Seccia S., Fidente P., Montesano D., Morrica P. Determination of neonicotinoid insecticides residues in bovine milk samples by solid-phase extraction clean-up and liquid chromatography with diode-array detection. J. Chromatogr. A., 2008, vol. 1214, pp. 115-120. doi:10.1016/j.chroma.2008.10.088.

Xie W., Han C., Qian Y., Ding H., Chen X., Xi J. Determination of neonicotinoid pesticides residues in agricultural samples by solid-phase extraction combined with liquid chromatography–tandem mass spectrometry. J. Chromatogr. A., 2011, vol. 1218, pp. 4426-4433. doi:10.1016/j.chroma.2011.05.026.

Pous X., Ruiz M.J., Pico Y., Font G. Determination of imidacloprid, metalaxyl, myclobutanil, propham, and thiabendazole in fruits and vegetables by liquid chromatography–atmospheric pressure chemical ionization–mass spectrometry. Fresenius J. Anal. Chem., 2001, vol. 371, pp. 182-189. doi: 10.1007/s002160100946.

Fernandez-Alba A.R., Tejedor A., Aguera A. Determination of imidacloprid and benzimidazole residues in fruits and vegetables by liquid chromatography–mass spectrometry after ethyl acetate multiresidue extraction. J. AOAC Int., 2000, vol. 83, no. 3, pp. 748-755.

Obana H., Okihashi M., Akutsu K., Kitagawa Y., Hori S. Determination of neonicotinoid pesticide residues in vegetables and fruits with solid phase extraction and liquid chromatography mass spectrometry. J. Agric. Food. Chem., 2003, vol. 51, pp. 2501-2505. doi: 10.1021/jf0261102.

Belen’kii B.G., Belov Iu.V., Kasalainen G.E. [High-performance capillary electrophoresis on environmental monitoring]. Z. Analit. Khimii. [J. Anal. Chem.], 1996, vol. 51, no. 8, pp. 817-834 (in Russian).

Komarova N.V., Kamentsev Ia.S. Prakticheskoe rukovodstvo po ispol'zovaniiu sistem kapilliarnogo elektroforeza «Kapel'» [Practical guidance on the use of capillary electrophoresis systems «Kapel»]. St. Petersburg: «Veda», 2006, 212 p (in Russian).

Segura Carretero A., Cruces-Blanco C., Perez Duran S., Fernandez Gutierrez A. Determination of imidacloprid and its metabolite 6-chloronicotinic acid in greenhouse air by application of micellar electrokinetic capillary chromatography with solid-phase extraction. J. Chromatogr. A., 2003, vol. 1003, pp. 189-195. doi: 10.1016 /S0021-9673(03)00835-5.

Amelin V.G., Bol'shakov D.S, Tret'iakov A.V. [Determination of neonicotiissids (imidacloprid, thiamethoxam, acetamiprid) in water by capillary electrophoresis]. Voda: khimiia i ekologiia [Water: Chemistry and Ecology], 2012, no. 9, pp. 76-80 (in Russian).

Schenck F.J., Hobbs J.E. Evaluation of the quick, easy, cheap, effective, rugged, and safe (QuEChERS) approach to pesticide residue analysis. Bull. Environ. Contam. Toxicol., 2004, vol. 73, no. 1, pp. 24-30. doi: 10.1007/s00128-004-0388-y.

Anastassiades M., Lehotay S.J., Stajnbaher D., Schenck F.J. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and «dispersive solid-phase extraction» for the determination of pesticide residues in produce. J. AOAC Int., 2003, vol. 86, no. 2, pp. 412-431.

Lehotay S.J., Son K.A., Kwon H., Koesukwiwat U., Fu W., Mastovska K., Hoh E., Leepipatpiboon N. Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables. J. Chromatogr. A., 2010, vol. 1217, pp. 2548-2560. doi: 10.1016/j.chroma.2010.01.044.


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