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采用同位素稀释-气相色谱/质谱法准确测定聚氯乙烯中 11 种代表性邻苯二甲酸酯和二(2-乙基己基)对苯二甲酸酯。

Accurate determination of 11 representative phthalates and di(2-ethylhexyl) terephthalate in polyvinyl chloride using isotope dilution-gas chromatography/mass spectrometry.

机构信息

Organic Metrology Group, Division of Chemical and Biological Metrology, Korea Research Institute of Standards and Science (KRISS), Daejeon 34113, Republic of Korea; Department of Chemistry, Chungnam National University, Daejon 34134, Republic of Korea.

Organic Metrology Group, Division of Chemical and Biological Metrology, Korea Research Institute of Standards and Science (KRISS), Daejeon 34113, Republic of Korea.

出版信息

J Chromatogr A. 2023 Nov 22;1711:464454. doi: 10.1016/j.chroma.2023.464454. Epub 2023 Oct 16.

Abstract

Phthalates are mainly used as plasticizers in polyvinyl chloride (PVC). However, prolonged exposure to phthalates poses considerable risks to human health. Consequently, the utilization of phthalates in consumer products is subject to regulations, with a defined threshold of 0.1 %. In this study, we developed an accurate and simultaneous method for determination of 11 representative phthalates and a non-phthalate plasticizer (di(2-ethylhexyl) terephthalate, DEHT) in PVC as a higher-order reference method. Homogeneously prepared PVC samples, each containing approximately 0.1 % of the target plasticizer compounds, were analyzed using gas chromatography-mass spectrometry (GC-MS) with deuterium-labeled phthalates and DEHT. The developed method could effectively separate and quantify all target plasticizers without interference with each other and potential overlap between the isomeric forms of phthalates, di-isodecyl phthalate, and di-isononyl phthalate. The developed method has high-order metrological quality, exhibiting exceptional selectivity, accuracy, repeatability (≤ 2.17 %), reproducibility (≤ 2.16 %), and relative expanded uncertainty (≤ 5.6 %). This analytical method is thus suitable for accurately assessing the target plasticizer levels in PVC products for ensuring compliance with the established 0.1 % threshold. This method was successfully applied to quantify twelve distinct plasticizers in PVC products obtained from the Korean market, validating its effectiveness and reliability in real-world scenarios.

摘要

邻苯二甲酸酯主要用作聚氯乙烯(PVC)的增塑剂。然而,长期接触邻苯二甲酸酯会对人类健康造成相当大的风险。因此,消费品中邻苯二甲酸酯的使用受到法规的限制,规定了 0.1%的限定阈值。在这项研究中,我们开发了一种准确且同时测定 11 种代表性邻苯二甲酸酯和一种非邻苯二甲酸酯增塑剂(对苯二甲酸二(2-乙基己基)酯,DEHT)的方法,作为一种高阶参考方法。使用气相色谱-质谱联用仪(GC-MS),对均匀制备的含有约 0.1%目标增塑剂化合物的 PVC 样品进行分析,其中使用氘标记的邻苯二甲酸酯和 DEHT。所开发的方法能够有效地分离和定量所有目标增塑剂,彼此之间没有干扰,也没有邻苯二甲酸酯、二异辛基邻苯二甲酸酯和二异壬基邻苯二甲酸酯的异构体形式之间的潜在重叠。所开发的方法具有高阶计量学质量,表现出优异的选择性、准确性、重复性(≤2.17%)、再现性(≤2.16%)和相对扩展不确定度(≤5.6%)。因此,该分析方法适用于准确评估 PVC 产品中目标增塑剂的水平,以确保符合既定的 0.1%阈值。该方法成功应用于量化从韩国市场获得的 PVC 产品中的十二种不同增塑剂,验证了其在实际情况下的有效性和可靠性。

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