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微波萃取/气质联用法测定细颗粒物(PM2.5)中邻苯二甲酸酯类化合物
Determination of Phthalate Esters in Particle Matter(PM2.5) by Microwave-assisted Extraction and Gas Chromatography- Mass Spectrometry
【摘要】 建立了环境空气细颗粒物(PM2.5)中痕量邻苯二甲酸酯类化合物(PAEs)的微波萃取(ME)/气相色谱-质谱联用(GC-MS)分析方法。样品经乙酸乙酯-丙酮混合溶剂微波提取后,经DB-5MS色谱柱分离,采用SCAN/SIM模式进行质谱测定,外标法定量。结果显示,PAEs的线性范围为100~1 000 pg,方法的检出限为0.101~0.262 ng/m3,加标回收率81.6%~129%。将本方法应用于常州化工园区环境空气细颗粒物中PAEs的分析检测发现,大部分PAEs在样品中检出,其中邻苯二甲酸二异丁酯(DIBP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二辛酯(DEHP)检出浓度较高,方法能够满足环境空气细颗粒物中痕量PAEs的测定要求。
【Abstract】 A simple method based on microwave extraction coupled with gas chromatography-mass spectrometry was developed for the determination of trace amounts of phthalates esters(PAEs) in environmental particle matter(PM2.5).The sample was extracted with ethyl acetate-acetone mixed solvent by microwave-assisted extraction.The PAEs were separated on a DB-5MS column and detected by MS under SCAN/SIM mode.The external standard method was used for the quantification.The linear ranges for the calibration curves of PAEs ranged from 100 pg to 1 000 pg.The limits of detection(MDL) ranged from 0.101 ng/m3to 0.262 ng/m3.The spiked recoveries were in the range of 81.6%-129%.The particle matters of ambient air in the Changzhou chemical industry park were successfully analyzed using the proposed method.15 PAEs were detected in the sample.The concentrations of diisobutyl phthalate(DIBP),dibutyl phthalate(DBP),dioctyl phthalate(DEHP) were high.The results showed that this would be a valuable method for the PAEs analysis in particle matter of ambient air.
【Key words】 microwave-assisted extraction; gas chromatography-mass spectrometry(GC-MS); phthalate esters(PAEs); particle matter(PM2.5);
- 【文献出处】 分析测试学报 ,Journal of Instrumental Analysis , 编辑部邮箱 ,2014年03期
- 【分类号】O657.63;X831
- 【被引频次】16
- 【下载频次】318