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

Emmanouil D Tsochatzis; Joao Alberto Lopes; Helen Gika; Trine Kastrup Dalsgaard; Georgios Theodoridis

doi:10.1016/j.foodchem.2021.129040

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

Food Chem. 2021 Jun 15:347:129040. doi: 10.1016/j.foodchem.2021.129040. Epub 2021 Jan 9.

Authors

Emmanouil D Tsochatzis¹, Joao Alberto Lopes², Helen Gika³, Trine Kastrup Dalsgaard⁴, Georgios Theodoridis⁵

Affiliations

¹ Department of Food Science, iFOOD, Centre for Innovative Food Research, Aarhus University, Agro Food Park 48, 8200 Aarhus N, Denmark. Electronic address: Emmanouil.Tsochatzis@food.au.dk.
² European Commission, Joint Research Centre, Geel, Belgium.
³ FoodOmicsGR Research Infrastructure, AUTh Node, Center for Interdisciplinary Research and Innovation (CIRI-AUTH), Balkan Center B1.4, 10th Km Thessaloniki-Thermi Rd, P.O. Box 8318, GR 57001 Thessaloniki, Greece; Biomic AUTh, Center for Interdisciplinary Research and Innovation (CIRI-AUTH), Balkan Center B1.4, 10th Km Thessaloniki-Thermi Rd, P.O. Box 8318, GR 57001 Thessaloniki, Greece; Department of Medicine, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece.
⁴ Department of Food Science, iFOOD, Centre for Innovative Food Research, Aarhus University, Agro Food Park 48, 8200 Aarhus N, Denmark.
⁵ FoodOmicsGR Research Infrastructure, AUTh Node, Center for Interdisciplinary Research and Innovation (CIRI-AUTH), Balkan Center B1.4, 10th Km Thessaloniki-Thermi Rd, P.O. Box 8318, GR 57001 Thessaloniki, Greece; Biomic AUTh, Center for Interdisciplinary Research and Innovation (CIRI-AUTH), Balkan Center B1.4, 10th Km Thessaloniki-Thermi Rd, P.O. Box 8318, GR 57001 Thessaloniki, Greece; Department of Chemistry, Aristotle University of Thessaloniki, 54124 Thessaloniki, Greece.

PMID: 33484960
DOI: 10.1016/j.foodchem.2021.129040

Abstract

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) 1^st 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 1^st series cyclic trimer was the most abundant oligomer, being found in all tested samples. The 1^st series PET cyclic dimer and tetramer, as well as 1,4,7-trioxacyclotridecane-8,13-dione, were found in considerable amounts. Traces of the 2^nd and 3^rd series PET cyclic dimers were also found.

Keywords: Analysis in food samples (pasta); Cyclic polyester oligomers; Food contact materials (FCM); Quadropole time of flight Mass Spectrometry (qTOF-MS); QueChERS clean-up method; Ultra High Performance Liquid chromatography (UHPLC).

MeSH terms

Aluminum Oxide / chemistry
Chromatography, High Pressure Liquid
Dimerization
Flour / analysis
Food Analysis / methods*
Mass Spectrometry / methods*
Polyesters / analysis
Polyesters / chemistry*
Polyethylene Terephthalates / analysis
Polyethylene Terephthalates / chemistry*
Polymerization
Silicon Dioxide / chemistry

Substances

Polyesters
Polyethylene Terephthalates
poly(1,4-butylene terephthalate)
Silicon Dioxide
Aluminum Oxide