This study aimed to develop a detection method of polyester oligomers in fatty food simulants.A total number of 7 polyester oligomers, including 4 polyethylene terephthalate (PET) oligomers and 3 polybutylene terephthalate (PBT) oligomers, were selected as target analytes.Olive oil was selected as a fatty food simulant.Sample pretreatment was carried out by using methanol (containing formic acid) as the extraction solvent and dichloromethane as an assistant extraction solvent.The procedures include vortexing, centrifugation, passing through the C18 cartridge, nitrogen blowing, and redissolution by ethanol.Detection of polyester oligomers was performed using liquid chromatography tandem mass spectrometry (LC-MS/MS).Results showed a good linear relationship of all polyester oligomers in the range of 10-500 μg/L (R2>0.99), with detection limits of 0.90-2.49 μg/L and quantification limits of 2.99-8.29 μg/L.Recovery of the 7 polyester oligomers locates in the range of 70%-120% at spike concentrations of 50, 100, 200, 500, and 1 000 μg/kg, with relative standard deviation of <12%.In summary, a simple and sensitive method for the detection of polyester oligomers in olive oil was developed.The detection method can be used in the migration testing of polyester oligomers from food contact materials, and provide technical support for the establishment of related standards.
[1] ZHANG M Y, BIESOLD G M, CHOI W, et al.Recent advances in polymers and polymer composites for food packaging[J].Materials Today, 2022, 53(Suppl C):134-161.
[2] ABID U, SUN G, SOONG Y H V, et al.Evaluation of enzymatic depolymerization of PET, PTT, and PBT polyesters[J].Biochemical Engineering Journal, 2023, 199:109074.
[3] OUYANG X Y, LU Z C, HU Y L, et al.Research progress on sample pretreatment methods for migrating substances from food contact materials[J].Journal of Separation Science, 2021, 44(4):879-894.
[4] SHIN C, KIM D G, KIM J H, et al.Migration of substances from food contact plastic materials into foodstuff and their implications for human exposure[J].Food and Chemical Toxicology, 2021, 154:112373.
[5] COLOMBO G, CORREDIG M, UYSAL ÜNALAN I, et al.Untargeted screening of NIAS and cyclic oligomers migrating from virgin and recycled polyethylene terephthalate (PET) food trays[J].Food Packaging and Shelf Life, 2024, 41:101227.
[6] HOPPE M, DE VOOGT P, FRANZ R.Identification and quantification of oligomers as potential migrants in plastics food contact materials with a focus in polycondensates-A review[J].Trends in Food Science & Technology, 2016, 50:118-130.
[7] UBEDA S, AZNAR M, NERÍN C.Determination of oligomers in virgin and recycled polyethylene terephthalate (PET) samples by UPLC-MS-QTOF[J].Analytical and Bioanalytical Chemistry, 2018, 410(9):2377-2384.
[8] UBEDA S, AZNAR M, ROSENMAI A K, et al.Migration studies and toxicity evaluation of cyclic polyesters oligomers from food packaging adhesives[J].Food Chemistry, 2020, 311:125918.
[9] TSOCHATZIS E D, ALBERTO LOPES J, KAPPENSTEIN O, et al.Quantification of PET cyclic and linear oligomers in teabags by a validated LC-MS method-In silico toxicity assessment and consumer's exposure[J].Food Chemistry, 2020, 317:126427.
[10] BRENZ F, LINKE S, SIMAT T J. Linear and cyclic oligomers in PET, glycol-modified PET and TritanTM used for food contact materials. Food Additives & Contaminants. Part A, Chemistry, Analysis, Control, Exposure & Risk Assessment, 2021, 38(1):160-179.
[11] BRENZ F, LINKE S, SIMAT T.Linear and cyclic oligomers in polybutylene terephthalate for food contact materials[J].Food Additives & Contaminants.Part A, Chemistry, Analysis, Control, Exposure & Risk Assessment, 2018, 35(3):583-598.
[12] XU T T, QIU K, GAO H B, et al.Simultaneous determination of cyclic PET and PBT oligomers migrated from laminated steel cans for food[J].Food Control, 2021, 130:108396.
[13] 吴刚, 潘家杰, 徐彤彤, 等.覆膜铁罐装食品中聚对苯二甲酸乙二醇酯及聚对苯二甲酸丁二酯环状低聚物的测定研究[J].食品与发酵工业, 2023, 49(19):312-318.
WU G, PAN J J, XU T T, et al.Determination of polyethylene terephthalate and polybutylene terephthalate cyclic oligomers in laminated steel canned food[J].Food and Fermentation Industries, 2023, 49(19):312-318.
[14] 王全新, 赵丹, 张宇含, 等.迁移至食品中的覆膜铁容器低聚物的检测方法[J].中国口岸科学技术, 2023, 5(6):21-29.
WANG Q X, ZHAO D, ZHANG Y H, et al.Detection method of oligomers migrating from laminated steel food containers to food[J].China Port Science and Technology, 2023, 5(6):21-29.
[15] 李倩云, 吴刚, 王亚, 等.覆膜金属罐中PBT/PET环状低聚物在食品中的迁移测试及基于膳食暴露量的风险评估[J].分析测试学报, 2022, 41(10):1494-1500.
LI Q Y, WU G, WANG Y, et al.Migration test and risk assessment based on dietary exposure of PBT/PET cyclic oligomers in polymer-laminated metal cans[J].Journal of Instrumental Analysis, 2022, 41(10):1494-1500.
[16] ALBERTO LOPES J, TSOCHATZIS E D, KARASEK L, et al.Analysis of PBT and PET cyclic oligomers in extracts of coffee capsules and food simulants by a HPLC-UV/FLD method[J].Food Chemistry, 2021, 345:128739.
[17] TSOCHATZIS E D, ALBERTO LOPES J, GIKA H, et al.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[J].Food Chemistry, 2021, 347:129040.
[18] FRANZ R, WELLE F.Migration measurement and modelling from poly (ethylene terephthalate) (PET) into soft drinks and fruit juices in comparison with food simulants[J].Food Additives & Contaminants. Part A, Chemistry, Analysis, Control, Exposure & Risk Assessment, 2008, 25(8):1033-1046.
[19] ÚBEDA S, AZNAR M, VERA P, et al.Overall and specific migration from multilayer high barrier food contact materials-kinetic study of cyclic polyester oligomers migration[J].Food Additives & Contaminants. Part A, Chemistry, Analysis, Control, Exposure & Risk Assessment, 2017, 34(10):1784-1794.
[20] HOPPE M, FORNARI R, DE VOOGT P, et al.Migration of oligomers from PET:Determination of diffusion coefficients and comparison of experimental versus modelled migration[J].Food Additives Contaminants.Part A, Chemistry, Analysis, Control, Exposure & Risk Assessment, 2017, 34(7):1251-1260.
