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一次性移液器萃取(DPX)的新策略:用于气相色谱-质谱法测定邻苯二甲酸酯从常见塑料材料向唾液模拟物迁移的低成本并行DPX。

Novel strategy for disposable pipette extraction (DPX): Low-cost Parallel-DPX for determination of phthalate migration from common plastic materials to saliva simulant with GC-MS.

作者信息

Huelsmann Ricardo Dagnoni, Will Camila, Carasek Eduardo

机构信息

Departamento de Química, Universidade Federal de Santa Catarina, Florianópolis, 88040900, Brazil.

Departamento de Química, Universidade Federal de Santa Catarina, Florianópolis, 88040900, Brazil.

出版信息

Talanta. 2021 Jan 1;221:121443. doi: 10.1016/j.talanta.2020.121443. Epub 2020 Aug 1.

DOI:10.1016/j.talanta.2020.121443
PMID:33076068
Abstract

In widespread use in commercial products as plasticizers, phthalic acid esters (phthalates) have worried researchers and society in general, given the negative impacts on living organisms, especially human health. Since they are not chemically linked to the polymeric matrix, their migration is evident for samples that come into contact with plastics that contain them, such as water, food and saliva. In this work, a new strategy is described, named parallel-disposable pipette extraction (Pa-DPX), in a fast, efficient and robust analytical method using five simultaneous extractions for the determination of migration of 6 phthalates from common plastic materials (children's toys, school supplies, dog toys and oral contact items) to saliva simulant, using gas chromatography-mass spectrometry (GC-MS). The optimized conditions were 5 extraction cycles with 1600 μL of saliva simulant and desorption with 200 μL of ethyl acetate using 5 cycles with the same aliquot. The calibration curves resulted in determination coefficients higher than 0.9915, limits of detection at 1.5 μg L, and the quantification limits were 5.0 μg L. Excellent results were obtained for repeatability (relative standard deviation ranging from 8.7% to 20.1% for 5 μg L) and intermediate precision, varying the day of analyses (7.9%-16.2%). The analyte recovery ranged from 75% to 114% for two different samples, in four different levels of concentration. The Pa-DPX-GC-MS method was successfully applied to determine the migration of PAE from 21 samples. At least one PAE was detected in 81% of samples, and di-n-octyl phthalate was found in higher concentration, achieving the migration of almost 30 μg per g of sample.

摘要

邻苯二甲酸酯作为增塑剂广泛应用于商业产品中,鉴于其对生物体尤其是人类健康的负面影响,一直令研究人员和整个社会担忧。由于它们与聚合物基体没有化学连接,对于与含有它们的塑料接触的样品,如水、食物和唾液,其迁移现象很明显。在这项工作中,描述了一种新策略,称为平行一次性移液器萃取(Pa-DPX),它是一种快速、高效且稳健的分析方法,采用五次同时萃取,使用气相色谱-质谱联用仪(GC-MS)测定六种邻苯二甲酸酯从常见塑料材料(儿童玩具、学习用品、宠物玩具和口腔接触物品)向唾液模拟物中的迁移情况。优化条件为使用1600μL唾液模拟物进行5次萃取循环,并用200μL乙酸乙酯使用相同等分试样进行5次循环解吸。校准曲线的测定系数高于0.9915,检测限为1.5μg/L,定量限为5.0μg/L。在重复性(5μg/L时相对标准偏差范围为8.7%至20.1%)和中间精密度(分析日期不同时为7.9%-16.2%)方面均获得了优异结果。对于两种不同样品在四种不同浓度水平下,分析物回收率范围为75%至114%。Pa-DPX-GC-MS方法成功应用于测定21个样品中邻苯二甲酸酯的迁移情况。81%的样品中至少检测到一种邻苯二甲酸酯,且邻苯二甲酸二正辛酯浓度较高,每克样品的迁移量几乎达到30μg。

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