Development and validation of an UHPLC-qTOF-MS method for the quantification of cyclic polyesters oligomers in pasta by applying a modified QuEChERS clean-up

• Published in: Food chemistry Vol. 347; p. 129040
• Main Authors: Tsochatzis, Emmanouil D., Alberto Lopes, Joao, Gika, Helen, Kastrup Dalsgaard, Trine, Theodoridis, Georgios
• Format: Journal Article
• Language: English
• Published: England Elsevier Ltd 15.06.2021
• Subjects: Aluminum Oxide - chemistry; Analysis in food samples (pasta); Chromatography, High Pressure Liquid; Cyclic polyester oligomers; Dimerization; Flour - analysis; Food Analysis - methods; Food contact materials (FCM); Mass Spectrometry - methods; Polyesters - analysis; Polyesters - chemistry; Polyethylene Terephthalates - analysis; Polyethylene Terephthalates - chemistry; Polymerization; Quadropole time of flight Mass Spectrometry (qTOF-MS); QueChERS clean-up method; Silicon Dioxide - chemistry; Ultra High Performance Liquid chromatography (UHPLC); QueChERS clean-up method; Food contact materials (FCM); Cyclic polyester oligomers; Quadropole time of flight Mass Spectrometry (qTOF-MS); Analysis in food samples (pasta); Ultra High Performance Liquid chromatography (UHPLC)
• ISSN: 0308-8146; 1873-7072
• DOI: 10.1016/j.foodchem.2021.129040

•Fast UHPLC-qTOF-MS analytical method.•Analysis of selected polyester cyclic oligomers.•Oligomers resulting from polyester food contact materials (FCM)•Method development and validation.•QueChERS clean-up with alumina (Al2O3) and primary secondary amine (PSA).•Applicability of the method to real food (pasta). An Ultra High-Performance Liquid chromatography method quadruple time-of-flight mass spectrometry has been developed for the analysis of 11 cyclic polyesters oligomers, following a modified QuEChERS clean-up with alumina/primary secondary amine, in pasta. Target analytes were polyethylene terephthalate (PET) 1st series cyclic dimer to heptamer, polybutylene terephthalate (PBT) dimer to pentamer and a polyurethane oligomer. Standard addition method was applied for the calibration, and the limits of quantification ranged from 3.2 to 17.2 ng g−1. Recoveries ranged from 86.4 to 109.8%, RSDs were lower than 12% for all analytes, and matrix effect never exceeded ± 2.5%. The method was successfully applied to real commercial pasta samples, where the PET 1st series cyclic trimer was the most abundant oligomer, being found in all tested samples. The 1st series PET cyclic dimer and tetramer, as well as 1,4,7-trioxacyclotridecane-8,13-dione, were found in considerable amounts. Traces of the 2nd and 3rd series PET cyclic dimers were also found.