Fabric phase sorptive extraction for specific migration analysis of oligomers from biopolymers

Oligomers are potential migrants from polymers or biopolymers intended to food packaging and they have to be under control. In order to comply with European regulation 10/2011, their concentration in migration must be below 0.01 μg g^-1. In this work, fabric phase sorptive extraction (FPSE) was explored as an effective method for extraction and pre-concentration of oligomers migrated from a blend PLA-polyester material. Both food simulant B (3% acetic acid) and juice, as real food, were used for migration experiments. The parameters of FPSE were optimized and the analysis was done by UHPLC-QTOF and UHPLC-QqQ. A total of 21 oligomers were identified, 9 of them coming from PLA and 12 oligomers from the polyester part. These oligomers were formed by adipic acid (AA), phthalic acid (PA) and/or butanediol (BD), ten were cyclic and 11 were linear molecules. Using the optimized FPSE procedure in 3% acetic acid as food simulant, it was possible to identify 3 new compounds that were not detected by direct injection of the simulant into UHPLC-QTOF. In addition, 2 extra compounds, cyclic PA-BD₄-AA₃ and cyclic PA₂-BD₃-AA, were only identified in juice samples after FPSE extraction. Besides, in order to quantify the compounds identified, an isolation procedure for PLA oligomers was carried out. Two oligomers were isolated: cyclic (LA)₆ and linear HO-(LA)₄-H, both with a purity higher than 90% (LA: lactic acid). The highest concentration value was found for the cyclic oligomer [AA-BD]₂, that showed 22.63 μg g^-1 in 3% acetic acid and 19.64 μg g^-1 in juice. The concentration of the total amount of remaining oligomers was below 7.56 μg g^-1 in 3% acetic acid as well as in juice.