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

作　　者：戴玄吏 李丹[2] 章霖之 蒋少杰 余益军 王延军 董黎静 

机构地区：[1]常州市环境监测中心,江苏常州213001 [2]常州大学环境与安全工程学院,江苏常州213001

出　　处：《分析测试学报》2014年第3期349-353,共5页Journal of Instrumental Analysis

基　　金：江苏省环保厅科技项目(201127);常州市科技项目(CE20125016)

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）的微波苯取（ME）/气相色谱-质谱联用（CC-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 000pg,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.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 envi- ronmental particle matter（ PM2.5 ）. The sample was extracted with ethyl acetate - acetone mixed sol- vent 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 detec- tion（MDL） ranged from 0. 101 ng/m3 to 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 con- centrations of diisobutyl phthalate （DIBP）, dibutyl phthalate （DBP）, dioetyl phthalate （DEHP） were high. The results showed that this would be a valuable method for the PAEs analysis in particle matter of ambient air.

关 键 词：微波萃取 气相色谱-质联谱用(GC-MS) 邻苯二甲酸酯类化合物 细颗粒物(PM2 5) 

分 类 号：O657.63[理学—分析化学] TQ414.1[理学—化学]