Department of Food Science, iFOOD, Centre for Innovative Food Research, Aarhus University, Agro Food Park 48, 8200 Aarhus N, Denmark.
European Commission, Joint Research Centre, Geel, Belgium.
Food Chem. 2021 Jun 15;347:129040. doi: 10.1016/j.foodchem.2021.129040. Epub 2021 Jan 9.
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 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. 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 series cyclic trimer was the most abundant oligomer, being found in all tested samples. The 1 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 and 3 series PET cyclic dimers were also found.
建立了一种超高效液相色谱-四极杆飞行时间串联质谱法，用于分析面食中 11 种环状聚酯低聚物，样品经改良的 QuEChERS 净化（氧化铝/伯仲胺）处理。目标分析物为聚对苯二甲酸乙二醇酯（PET）1 系列环状二聚体到七聚体、聚对苯二甲酸丁二醇酯（PBT）二聚体到五聚体和一种聚氨酯低聚物。采用标准加入法进行校准，定量限范围为 3.2-17.2ng/g。回收率为 86.4-109.8%，所有分析物的 RSD 均低于 12%，基质效应从不超过±2.5%。该方法成功应用于实际商业面食样品，其中 PET 1 系列环状三聚体是最丰富的低聚物，在所有测试样品中均有发现。1 系列 PET 环状二聚体和四聚体以及 1,4,7-三氧杂环十三烷-8,13-二酮含量相当高。还发现了痕量的 2 系列和 3 系列 PET 环状二聚体。
