Determination of pesticides in sunflower seeds by high-performance liquid chromatography coupled with a diode array detector

Abstract

The application of RP-HPLC with a diode array detector for identification and quantitative analysis of pesticides in sunflower seed samples is demonstrated. An HPLC procedure on C18 RP column has been developed for analysis of selected pesticides from different chemical groups: simazine, isoproturon, terbuthylazine, linuron, captan, terbutryn, procymidone, fenitrothion, clofentezine, and bromopropylate. We investigated the possibility of expanding the scope of the four analyte extraction procedures for isolation of pesticides from plant matrixes with high levels of lipids. The following procedures were tested: A, ultrasound-assisted solvent extraction (UAE) and SPE; B, dispersive-SPE (d-SPE); C, UAE and d-SPE; and D, UAE/SPE/d-SPE. Average recoveries from spiked samples at different concentrations in the range from 0.1 to 1.40 μg/g in the plant materials and the SDs for C18 cartridges and solvents by the proposed RP-HPLC-DAD method after the extraction procedures are also presented. The efficiency of procedures A-D was evaluated using real food samples from Hungary, Bulgaria, and Poland. The quantity of terbuthylazine determined was in the range of 7.1-12.7 ng/g (n = 6), whereas the quantity of procymidone determined was in the range of 3.7-5.7 ng/g (n = 3) in plant materials. The quantities of pesticides determined in sunflower seeds were below the maximum residue levels (excluding captan) established in the European Union legislation. The method was validated for precision and accuracy.