Determination of bisphenol-type endocrine disrupting compounds in food-contact recycled-paper materials by focused ultrasonic solid–liquid extraction and ultra performance liquid chromatography-high resolution mass spectrometry

Focused ultrasonic solid–liquid extraction (FUSLE) and reverse-phase ultra performance liquid chromatography (UPLC) coupled to a quadrupole-time of flight mass spectrometer (Q-TOF-MS) was applied to the determination of bisphenol-type endocrine disrupting compounds (EDCs) in food-contact recycled-paper materials. Recycled paper is a potential source of EDCs. Bisphenol A (BPA), bisphenol F (BPF) and their derivatives bisphenol A diglycidyl ether (BADGE) and bisphenol F diglycidyl ether (BFDGE) are used for the production of epoxy resins employed in the formulation of printing inks. The FUSLE of bisphenol-type EDCs from packaging is reported for the first time. First, different extraction solvents were studied and methanol was selected. Then, the main FUSLE factors affecting the extraction efficiency (solvent volume, extraction time and ultrasonic irradiation power) were studied by means of a central composite design. The FUSLE conditions selected for further experiments were 20ml of methanol at ultrasonic amplitude of 100% for 5s. Finally, the number of extraction cycles necessary for complete extraction was established in two. The analysis of the FUSLE extracts was carried out by UPLC-Q-TOF-MS with electrospray ionization and the determination of the four analytes took place in only 4min. The FUSLE and UPLC-ESI-QTOF-MS method was validated and applied to the analysis of different food-contact recycled-paper-based materials and packaging. The proposed method provided recoveries from 72% to 97%, repeatability and intermediate precision under 9% and 14%, respectively, and detection limits of 0.33, 0.16, 0.65 and 0.40μg/g for BPA, BPF, BADGE and BFDGE, respectively. The analysis of paper and cardboard samples confirmed the presence of EDCs in these packaging. ► FUSLE and UPLC-HRMS determination of four endocrine disrupters in paper and cardboard. ► Analytes are bisphenol A, bisphenol F and their diglycidyl ether derivatives. ► Complete extraction in two FUSLE cycles of 5s and UPLC separation in only 4min. ► Presence of bisphenol A and F in different food-contact recycled-paper materials. ► Diglycidyl ether derivatives were not found in the analyzed samples.