色谱2025，Vol.43Issue(2)：185-196,12.DOI:10.3724/SP.J.1123.2023.12002
基于全二维气相色谱-飞行时间质谱分析室内灰尘中邻苯二甲酸酯及其新型替代品
Analysis of phthalate esters and their novel alternatives in indoor dust using comprehensive two-dimensional gas chromatography-time of flight mass spectrometry
摘要
Abstract
A comprehensive two-dimensional gas chromatography-time-of-flight mass spec-trometry(GCxGC-TOF-MS)method was developed to analyze 25 traditional phthalate esters(PAEs)and 19 novel alternatives in indoor dust samples.PAEs are ubiquitous in indoor envi-ronments because they are widely used as plasticizers in a variety of consumer products,and potential health concerns have prompted the need for effective monitoring methods.In this study,dust samples were collected from various indoor settings in a university campus,inclu-ding classrooms,cafeterias,laboratories,and dormitories,and were subsequently ultrasonically extracted with hexane-dichloromethane(1∶1,v/v)solution for 30 min.This method was chosen to maximize PAE recovery while minimizing potential interference from other compounds present in the dust matrix.Compounds were separated on a Rix-5MS column(30 m×0.25 mm×0.25 μm)as the first dimension,with a Rix-17Sil column(1.39 m×0.25 mm×0.25 μm)serving as the second dimension.The following temperature program was used:60 ℃ for 1 min,then increasing to 220 ℃ at 20 ℃/min,followed by a further increase to 290 ℃ at 5 ℃C/min,with the final temperature held for 8 min;this program was optimized to afford maxi-mum target-compound resolution and sensitivity.The developed method rapidly,accurately,and sensitively detected the target PAEs and their alternatives under the optimal conditions,which included a carrier-gas flow rate of 1.4 mL/min,a modulation period of 4 s,and an injec-tion-port temperature of 250 ℃C.The 44 target compounds exhibited highly linear calibration curves across a content range of 1-500 μg/g,with all correlation coefficients exceeding 0.99.The limits of detection(LODs)of the method were determined to lie between 0.57 and 13.0 ng/g,which reflects the high sensitivity of the developed approach.At spiked levels of 1,10,and 50 μg/g,the recoveries of the analyzed compounds varied from 72.8％to 125％,with rela-tive standard deviations ranging from 1.29％to 14.8％(n=3),which indicates that the method is highly precise and reliable.The developed method was used to analyze PAEs and their alter-natives in 40 indoor dust samples,which revealed total contents of between 2.07 and 354 μg/g in dust samples.Di-2-ethylhexyl phthalate(DEHP)emerged as the most frequently detected compound,with contents ranging from"not detected"(nd)to 158 μg/g.The novel alterna-tive,bis(2-ethylhexy)terephthalate(DEHTH),was also detected,with levels ranging from nd to 117 μg/g.Notably,significant differences in the compositions and contents of the PAEs and their alternatives were observed across various indoor environments,which suggests that di-verse sources and exposure pathways exist for these compounds,highlighting the necessity for ongoing PAE monitoring and risk assessment in various indoor settings.In conclusion,the de-veloped GCxGC-TOF-MS method provides a powerful tool for comprehensively analyzing PAEs and their alternatives in indoor dust;it is well-suited for the routine monitoring of these com-pounds owing to its simplicity,rapidity,and robustness.These findings provide valuable insight for future research into the sources and health implications of PAEs in indoor environments,and ultimately support risk assessment and regulatory efforts.关键词
全二维气相色谱-飞行时间质谱联用/邻苯二甲酸酯/室内灰尘/广谱筛查Key words
comprehensive two-dimensional gas chromatography-time of flight mass spectrom-etry(GCxGC-TOF-MS)/phthalates(PAEs)/indoor dust/broad spectrum screening分类
化学化工引用本文复制引用
王林啸,程水源,高珂,李建佳,彭佳慧,杨紫砚,牙尔肯,郑丛宜,魏巍,鲁理平..基于全二维气相色谱-飞行时间质谱分析室内灰尘中邻苯二甲酸酯及其新型替代品[J].色谱,2025,43(2):185-196,12.基金项目
国家自然科学基金(22206009) （22206009）
北京市自然科学基金(8232020).National Natural Science Foundation of China(No.22206009) （8232020）
Beijing Natural Science Foundation(No.8232020). （No.8232020）
