Generic sample treatment method for simultaneous determination of multiclass pesticides and mycotoxins in wines by liquid chromatography–mass spectrometry

In this work, a generic sample treatment method for simultaneous determination of multiclass pesticides and mycotoxins in wines is presented. The proposed method is based on solid-phase extraction (SPE) using polymeric-type SPE cartridges. To evaluate the proposed sample treatment, a liquid chromatography electrospray time-of-flight mass spectrometry method was used for testing 60 selected representative multiclass pesticides and 9 mycotoxins. Two different polymeric sorbents were evaluated, with hydrophilic–lipophilic-balanced (HLB) polymer cartridges being selected (Oasis™ HLB) as the most suitable for the present study. The identification and confirmation of the compounds was based on retention time and accurate mass measurements of the protonated molecules ([M+H]+). Limits of detection were below 1 μg L−1 for the 87% of the studied compounds. With the selected 4:1 preconcentration factor, 70% of the target compounds showed relatively low matrix effects, corresponding to signal suppressions lower than 30%. Recovery studies (n = 10) were carried out at two concentration levels, 2.5 μg L−1 and 25 μg L−1, obtaining mean recovery rates between 70 and 120% for the 90% of studied analytes. The relative standard deviation (RSD%) values of the entire procedure were below 15% in most cases (97% of the studied analytes). The proposed method was successfully applied to 24 red wine samples produced in different regions of Spain. The concentration levels of the target compounds found in the studied samples were in compliance with the current regulations. Aflatoxin B2 and metalaxyl were the most detected compounds (75% and 50% of the studied samples, respectively).

► Generic sample treatment for simultaneous determination of pesticides and mycotoxins in wines.
► An LC–TOFMS method was used for testing 69 selected representative multiclass contaminants.
► Two different polymeric sorbents were evaluated.
► The method was successfully applied to 24 Spanish red wine samples.
► Aflatoxin B2 and metalaxyl were the most often detected compounds.