Phthalic acid esters (PAEs) are a class of chemicals widely used as plasticizers. These compounds, considered toxic, do not bond to the polymeric matrix of plastic and can, therefore, migrate into the surrounding environment, posing a risk to human health. The primary source of human exposure is food, which can become contaminated during cultivation, production, and packaging. Therefore, it is imperative to control and regulate this exposure. This review covers the analytical methods used for their determination in two economically significant products: olive oil and wine. Additionally, it provides a summary and analysis of information regarding the characteristics, toxicity, effects on human health, and current regulations pertaining to PAEs in food. Various approaches for the extraction, purification, and quantification of these analytes are highlighted. Solvent and sorbent-based extraction techniques are reviewed, as are the chromatographic separation and other methods currently applied in the analysis of PAEs in wines and olive oils. The analysis of these contaminants is challenging due to the complexities of the matrices and the widespread presence of PAEs in analytical laboratories, demanding the implementation of appropriate strategies.
This study monitored the contamination of 32 plasticizers in olive oil throughout the production and storage process. Samples were collected at different stages of production from three olive oil production lines in distinct regions of Portugal and analyzed for 23 phthalates and 9 phthalates substitutes to identify contamination sources. The developed analytical method employed liquid–liquid extraction with hexane/methanol (1:4, v/v), followed by centrifugation, extract removal, and freezing as a clean-up step. Analysis was conducted using gas chromatography tandem mass spectrometry (GC-MS/MS), with detection limits ranging from 0.001 to 0.103 mg/kg. The results revealed that plasticizer concentrations progressively increased at each stage of the production process, although unprocessed olives also contained contaminants. Di-isononyl phthalate (DINP) was the most prevalent compound, but all phthalates regulated by the European Union for food contact materials were detected, as well as some unregulated plasticizers. In a few packaged olive oils, DINP concentrations exceeded the specific migration limits established by European regulations. Samples stored in glass and plastic bottles showed no significant differences in plasticizer concentrations after six months of storage. However, higher concentrations were observed in plastic-packaged samples after 18 months of storage. Our findings indicate that the primary source of plasticizer contamination in olive oil originates from the production process itself, except for prolonged storage in plastic bottles, which should be avoided.