热裂解气相色谱法快速筛查高分子材料中4种邻苯二甲酸酯类增塑剂

熊松松, 简佩玲, 孙秀敏, 郭范娟, 苏健梅, 丑天姝

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塑料科技 ›› 2025, Vol. 53 ›› Issue (02) : 136-141. DOI: 10.15925/j.cnki.issn1005-3360.2025.02.025
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热裂解气相色谱法快速筛查高分子材料中4种邻苯二甲酸酯类增塑剂

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Rapid Screening of Four Phthalate Ester Plasticizers in Polymeric Materials Using Pyrolyzer Gas Chromatography

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摘要

采用热裂解气相色谱法(Py-GC)建立了快速筛查高分子材料中4种邻苯二甲酸酯类化合物(PAEs)的分析方法。将样品粉碎研磨后,直接称取一定量样品,进样于热裂解邻苯检测仪进行分析,采用外标法定量分析,考察了取样量、温度等因素对回收率的影响,确定最佳前处理条件。结果表明:分析物在100~4 000 mg/kg浓度范围内线性关系良好(r 2>0.996 0),检出限为12.1~33.4 mg/kg。采用不同浓度的阳性物质分析方法的准确度和精密度,分析物的回收率为77.4%~125.5%,相对标准偏差为1.7%~12.8%。采用此方法对26个实际样品进行检测分析,在12个样品中检测出PAEs,检出率高达46%。该方法不使用化学试剂,直接对样品进行测试,能够满足企业对PAEs的快速筛查要求,为企业内部管控PAEs提供方法支持。

Abstract

A rapid screening method for the analysis of four phthalate esters (PAEs) in polymeric materials was established using pyrolysis gas chromatography (Py-GC). After grinding the samples into powder, a certain amount of the sample was directly weighed and injected into the pyrolysis phthalate detector for analysis. External standard method was used for quantitative analysis. Factors such as sample amount and temperature that affect the recovery rate were investigated, and the optimal pre-treatment conditions were determined. The results show that the analytes exhibited good linearity within the concentration range of 100~4 000 mg/kg (r²>0.996 0), with detection limits ranging from 12.1 to 33.4 mg/kg. The accuracy and precision of the method were evaluated using positive substances at different concentrations. The recovery rates of the analytes were between 77.4% and 125.5%, with relative standard deviations ranging from 1.7% to 12.8%. This method was applied to analyze 26 actual samples, and PAEs were detected in 12 of them, with a high detection rate of 46%. The method does not use chemical reagents and allows direct testing of samples, which can meet the requirements of enterprises for rapid screening of PAEs and provides a methodological support for internal control of PAEs within enterprises.

关键词

邻苯二甲酸酯 / 高分子材料 / 热裂解 / 快速筛查

Key words

Phthalate ester / Polymeric materials / Pyrolyzer / Rapid screening

中图分类号

O657.71

引用本文

导出引用
熊松松 , 简佩玲 , 孙秀敏 , . 热裂解气相色谱法快速筛查高分子材料中4种邻苯二甲酸酯类增塑剂. 塑料科技. 2025, 53(02): 136-141 https://doi.org/10.15925/j.cnki.issn1005-3360.2025.02.025
XIONG Songsong, JIAN Peiling, SUN Xiumin, et al. Rapid Screening of Four Phthalate Ester Plasticizers in Polymeric Materials Using Pyrolyzer Gas Chromatography[J]. Plastics Science and Technology. 2025, 53(02): 136-141 https://doi.org/10.15925/j.cnki.issn1005-3360.2025.02.025

参考文献

1
ZHAO A Q, WANG L X, PANG X Y, et al. Phthalates in skin wipes: Distribution, sources, and exposure via dermal absorption[J]. Environmental Research, 2022, 204: 112041.
2
孙春峰,秦芳.化妆品塑料包装中邻苯二甲酸酯含量的测定[J].塑料工业,2018,46(1):95-98.
3
NET S, SEMPÉRÉ R, DELMONT A, et al. Occurrence, fate, behavior and ecotoxicological state of phthalates in different environmental matrices[J]. Environmental Science & Technology, 2015, 49(7): 4019-4035.
4
ZHANG Z M, ZHANG H H, ZHANG J, et al. Occurrence, distribution, and ecological risks of phthalate esters in the seawater and sediment of Changjiang River Estuary and its adjacent area[J]. Science of the Total Environment, 2018, 619/620: 93-102.
5
KATSIKANTAMI I, SIFAKIS S, TZATZARAKIS M N, et al. A global assessment of phthalates burden and related links to health effects[J]. Environment International, 2016, 97(12): 212-236.
6
LIAO C X, LIU W, ZHANG J L, et al. Associations of urinary phthalate metabolites with residential characteristics, lifestyles, and dietary habits among young children in Shanghai, China[J]. Science of the Total Environment, 2018, 616-617: 1288-1297.
7
CAO Y R, LI J, WU R B, et al. Phthalate esters in seawater and sediment of the northern South China Sea: Occurrence, distribution, and ecological risks[J]. Science of The Total Environment, 2022, 811: 151412.
8
LIU H, CUI K Y, ZENG F, et al. Occurrence and distribution of phthalate esters in riverine sediments from the Pearl River Delta region, South China[J]. Marine Pollution Bulletion, 2014, 83(1): 358-365.
9
RAMZI A, GIREESHKUMAR T R, HABEEB RAHMAN K, et al. Distribution and contamination status of phthalic acid esters in the sediments of a tropical monsoonal estuary, Cochin-India[J]. Chemosphere, 2018, 210: 232-238.
10
SONG M, CHI C C, GUO M, et al. Pollution levels and characteristics of phthalate esters in indoor air of offices[J]. Journal of Environmental. Sciences (China), 2015, 28: 157-162.
11
XU W H, YOU Y M, WANG Z G, et al. Dibutyl phthalate alters the metabolic pathways of microbes in black soils[J]. Scientific Reports, 2018, 8(1): 2605.
12
CHEN Y L, WANG Y L, TAN Y, et al. Phthalate esters in the Largest River of Asia: An exploration as indicators of microplastics[J]. Science of The Total Environment, 2023, 902: 166058.
13
PALUSELLI A, AMINOT Y, GALGANI F, et al. Occurrence of phthalate acid esters (PAEs) in the northwestern Mediterranean Sea and the Rhone River[J]. Progress in Oceanography, 2018, 163: 221-231.
14
SICIŃSKA P, JABŁOŃSKA E, BUKOWSKA B, et al. The selected epigenetic effects of phthalates: DBP, BBP and their metabolites: MBP, MBzP on human peripheral blood mononuclear cells (In Vitro)[J]. Toxicology in Vitro, 2022, 82: 105369.
15
WU Y D, SONG J, LI Y X, et al. Association between exposure to a mixture of metals, parabens, and phthalates and fractional exhaled nitric oxide: A population-based study in US adults[J]. Environmental Research, 2022, 214: 113962.
16
AIMUZI R, WANG Y Q, LUO K, et al. Exposure to phthalates, phenols, and parabens mixture and alterations in sex steroid hormones among adolescents[J]. Chemosphere 2022, 302: 134834.
17
YANG M, CHEN Z, CAO Z Q, et al. Prenatal exposure to phthalates and child growth trajectories in the first 24 months of life[J]. Science of The Total Environment, 2023, 898: 165518.
18
XIE M J, WU Y X, LITTLE J C, et al. Phthalates and alternative plasticizers and potential for contact exposure from children's backpacks and toys[J]. Journal of Exposure Science & Environmental Epidemiology, 2016, 26(1): 119-124.
19
AXELSSON J, RYLANDER L, RIGNELL-HYDBOM A, et al. Phthalate exposure and reproductive parameters in young men from the general Swedish population[J]. Environment International, 2015, 85(12): 54-60.
20
ZENG H H, ZHANG H X, WU X, et al. Pollution levels and health risk assessment of particulate phthalic acid esters in arid urban areas[J]. Atmospheric Pollution Research, 2017, 8(1): 188-195.
21
李蔚,吴楠,田冲,等.高效液相色谱-质谱联用法测定塑料包书皮中邻苯二甲酸酯类物质[J].中国口岸科学技术,2022(04):74-79.
22
国家市场监督管理总局,国家标准化管理委员会. 电子电气产品中某些物质的测定第8部分:气相色谱-质谱法(GC-MS)与配有热裂解/热脱附的气相色谱-质谱法(Py/ TD-GC-MS)测定聚合物中的邻苯二甲酸酯:GB/T 39560.8—2021[S].北京:中国标准出版社,2021.
23
何芃.气相色谱-质谱法同时测定橡塑材料中18种邻苯二甲酸酯类增塑剂[J].塑料工业,2010,38(9):60-64.
24
白荣汉.气质联用法测定塑料快递袋中18种邻苯二甲酸酯含量[J].塑料科技,2022,50(9):80-84.
25
国家市场监督管理总局,国家标准化管理委员会. 电子电气产品中某些物质的测定第3-1部分:X射线荧光光谱法筛选铅、汞、镉、总铬和总溴:GB/T 39560.301—2020 [S].北京:中国标准出版社,2020.
26
中华人民共和国国家质量监督检验检疫总局. 电子电气产品中多溴联苯和多溴二苯醚的测定 第2部分 红外光谱定性筛选法:SN/T 2003.2—2006 [S].北京:中国标准出版社,2006.

基金

广州市增城区科技计划项目(2024ZCKJ11)

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