Determination of phthalate esters in wine using solid-phase extraction and gas chromatography–mass spectrometry

A method for the determination of six phthalate esters in wine samples has been developed. The phthalates were extracted from wine samples with an optimised solid-phase extraction method on C18 column and quantification was achieved via gas chromatography coupled with a mass spectrometer. The method was linear between 0.015 and 5.000 μg mL−1 for DMP, DEP and DEHP and between 0.018 and 5.000 μg mL−1 for iBP, DBP and BBP. The LOQs of DMP, DEP and DEH were 0.024 μg mL−1 while those of iBP, DBP and BBP were 0.029 μg mL−1. The intra-day method repeatability was between 10% and 15% RSD, whereas the inter-day method repeatability was between 13% and 21% RSD. A survey was performed on white and red wines (n = 62) from the market, winemakers and an experimental pilot plant. All the analysed samples were phthalate contaminated. Commercial wine showed higher detection frequency and level of total phthalate, DBP and BBP than those produced in a pilot plant. iBP and DEHP concentrations were similar in all the groups of samples. iBP concentration was higher in red wines than in white ones.