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


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




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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