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基于全链条的回收PET材料中非挥发性可迁移物的非靶向筛查及特征风险标志物的确定
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作者单位
杨颉,马鑫,杨道远,隋海霞,杜振霞 1. 北京化工大学 化学学院北京 100029 2. 国家食品安全风险评估中心北京 100022 
基金项目:国家重点研发计划(2019YFC1606502);国家自然科学基金(32061160474)
中文摘要:基于超高效液相色谱-四极杆飞行时间质谱(UPLC-Q-TOF MS)对回收聚对苯二甲酸乙二醇酯(回收PET,rPET)全链条中回收碎片及由碎片造粒得到的粒料、瓶坯、瓶子4个阶段rPET样品进行溶解沉淀实验及模拟迁移试验,对样品中的潜在迁移物及迁移物进行非靶向筛查,得到包括PET寡聚体、润滑剂、漂洗剂在内的30种有意、非有意添加物。使用MS-DIAL(Mass spectrometry-data independent analysis software)软件对rPET不同生产阶段的产品标志物进行快速筛选,发现在粒料到瓶坯的加工过程中,生成了新的PET寡聚体;rPET碎片样品中标志物为脂肪醇聚氧乙烯醚,分析可能由漂洗过程引入。对比PET寡聚体的相对含量发现,rPET材料中环状寡聚体的相对含量高于线性寡聚体,其中第二系列环状二聚体的相对含量最高。在rPET加工过程中部分寡聚体及润滑剂的相对含量增加。最后通过TEST(Toxicity estimation software tool)软件预测潜在迁移物及迁移物的大鼠经口急性毒性、发育毒性和致突变性,采用Toxtree软件进行Cramer分级,PET环状寡聚体及酰胺类润滑剂均被分为Cramer Ⅲ级,毒性均高于线性寡聚体,应在rPET加工过程中引起关注。
中文关键词:回收PET  食品接触材料  超高效液相色谱-四极杆飞行时间质谱  MS-DIAL  风险评估
 
Non-targeted Screening of Nonvolatile Migration Compounds in Recycled PET Based on Whole Chain and Their Identification of Characteristic Risk Markers
Abstract:Based on the whole chain of recycled polyethylene terephthalate(recycled PET,rPET),potential migrants in recycled flakes,pellets,preforms and bottles/migrants in the food simulation solution were untargeted screened by ultrahigh performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF MS).Thirty kinds of intentionally or non-intentionally added substances including PET oligomers,lubricants and rinsing agents were screened out.MS-DIAL(Mass spectrometry-data independent analysis software) was employed to screen the markers of rPET products in different production stages.The results showed that new PET oligomers were formed during the processing from pellet to preform.Alcohol ethoxylate was detected in the flakes of rPET due to the clean process.Comparing the relative content of PET oligomers,it was found that the relative content of cyclic oligomers in rPET was higher than that of linear oligomers,while the relative content of the second series of cyclic dimers was the highest.The relative content of several kinds of oligomers and lubricants increased during rPET processing.Finally,the TEST(Toxicity estimation software tool) was used to predict the rat oral acute toxicity,developmental toxicity and Ames mutagenicity of potential migrants/migrants.And the classification of potential migrants/migrants by Cramer rules was performed by Toxtree software. It was found that PET cyclic oligomers and amide lubricants were all classified as Cramer Ⅲ,which was more toxic than linear oligomers,suggesting that attention should be paid during the rPET recycling process.
Key Words:recycled PET  food contact materials  ultrahigh performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry  MS-DIAL  risk assessment
引用本文:杨颉,马鑫,杨道远,隋海霞,杜振霞.基于全链条的回收PET材料中非挥发性可迁移物的非靶向筛查及特征风险标志物的确定[J].分析测试学报,2021,40(11):1553-1560.
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