Analysis of post-harvest fungicides by micellar electrokinetic chromatography

A method based on solid-phase extraction (SPE) and micellar electrokinetic chromatography (MEKC) was developed for the simultaneous determination of carbendazim, imazalil, methylthiophanate, O-phenylphenol, prochloraz, procimidone, thiabendazole and triadimefon residues in grape, lettuce, orange and tomato. Selectivity and resolution were studied changing the pH and the concentration of the buffer, the type and concentration of surfactant and the methanol content in the mobile phase. A buffer consisting of 4 mM borate with 75 mM sodium cholate (pH 9.2) gave the best results. The recoveries of the fungicides in spiked fruit and vegetable samples ranged from 30 to 105%, and the limits of detection were between 0.1 and 1 mg kg−1. The reproducibility and repeatability of the combination of SPE pretreatment and MEKC were good for all the compounds, except for imazalil and O-phenylphenol in oranges, due to some matrix compounds interfering with the separation. The method was applied to post harvest treated samples, and the fungicides were sometimes detected at concentration levels lower than maximum residue limits (MRLs).