摘要
目的通过自行制备阳性样品的方式,研究聚氯乙烯塑料(PVC)塑料中乙酰柠檬酸三丁酯的(ATBC)添加量、残留量和迁移量三者间的关系,为有效控制PVC中ATBC的安全风险提供技术支持。方法为准确测试PVC垫片中ATBC的残留量,首先建立溶解-沉淀-气相色谱-质谱检测方法,样品经四氢呋喃溶解后,加入乙腈沉淀溶液中的大分子化合物,再将清液用GC-MS法测定,得到PVC中ATBC的残留量,并对ATBC残留量方法进行方法学验证。PVC中ATBC迁移量的测定采用已有文献的方法。对自行制备的分别添加了2%、5%、10%、20%、30%、40%、50%ATBC的PVC塑料垫片分别进行残留量和迁移量测试,研究添加量、残留量和迁移量三者之间的关系。结果新建立的ATBC残留量检测方法在0.20~5.0 mg/L范围内线性关系良好,相关系数达0.998,方法检出限为5 mg/kg,定量限为20.0 mg/kg,加标回收率为95.6%~102%,相对标准偏差(n=6)为3.7%~6.8%。对自行加工的阳性样品进行残留量和迁移量测试,发现ATBC残留量和迁移量均与添加量呈显著的正相关性。当添加量处于相同水平时,ATBC在4%乙酸和20%乙醇中的迁移水平较低,而在橄榄油和异辛烷中的迁移水平较高。当ATBC的添加量达到30%时,其在橄榄油和异辛烷中的迁移风险已接近超标水平,需引起关注;当添加量达到50%时,在橄榄油和异辛烷中的迁移量超过限量要求。结论本研究将为瓶盖用PVC垫片的生产企业科学控制ATBC添加量,做好ATBC迁移量的合规管控提供科学的数据支持。
The work aims to study the relationship between the addition amount,residual amount,and migration amount of acetyl tributyl citrate(ATBC)in polyvinyl chloride(PVC)plastics by preparing positive samples so as to provide technical support for production enterprises to effectively control the safety risks of ATBC in PVC.To accurately test the residual amount of ATBC in PVC gaskets,a dissolution precipitation gas chromatography-mass spectrometry detection method was first established.After dissolving the sample in tetrahydrofuran,the large molecular compounds in the acetonitrile precipitation solution were added,and the clear solution was determined by GC-MS to obtain the residual amount of ATBC in PVC.Using literature review methods,the migration amount of ATBC in different food simulants in the sample was determined.Residual and migration tests were conducted on PVC plastic gaskets prepared by ourselves with 2%,5%,10%,20%,30%,40%,and 50%ATBC added.The methodological validation of the newly established ATBC residue determination method showed a good linear relationship and correlation coefficient within the range of 0.20-5.0 mg/L,the correlation coefficient reached 0.998.The residue method detection limit was 5.0 mg/kg and quantification limit was 20 mg/kg,the spiked recovery rate was 95.6%-102%,and the relative standard deviation(n=6)was 3.7%-6.8%.The residue and migration test of positive samples processed by themselves showed that the residue and migration of ATBC were significantly positively correlated with the addition amount.When addition amount was at the same level,the migration level of ATBC in 4%acetic acid and 20%ethanol was low,while the migration level in olive and isooctane was high.When the addition amount of ATBC reached 30%,its migration risk in olive oil and isooctane approached the overstandard level,which needed to be concerned.When the addition amount reached 50%,the migration amount in olive oil and isooctane exceeded the limit requirement.This research will provide scientific data support for the scientific control of the addition amount of ATBC and the compliance control of the migration amount of ATBC in the production enterprises of PVC gaskets for caps.
作者
陈湘颖
谢苍昊
秦简
周建安
潘迎春
阿文伟
李丹
CHEN Xiangying;XIE Canghao;QIN Jian;ZHOU Jianan;PAN Yingchun;A Wenwei;LI Dan(Guangzhou Customs Technical Center,Guangzhou 510275,China;Wuxi Huapeng Closures Co.,Ltd.,Jiangsu Wuxi 214142,China;Lemon-flex Company Limited China,Jiangsu Yixing 214213,China)
出处
《包装工程》
北大核心
2025年第15期177-183,共7页
Packaging Engineering
基金
海关总署科研项目(2024HK273)。
