电喷雾萃取电离质谱法直接检测环境水样中的邻苯二甲酸二(2-乙基己基)酯  

Direct Detection of Di-2-ethylhexy Phthalate in Environmental Water Sample Based on Extractive Electrospray Ionization Mass Spectrometry

作　　者：梁大鹏 方媛萍 刘文杰 张华[2] 裘彦挺 董祎铭 宁杨 LIANG Da-Peng1, FANG Yuan-Ping1, LIU Wen-Jie1 , ZHANG Hua2, QIU Yan-Ting1 , DONG Yi-Ming1 , NING Yang1(1 College of Environment and Resources, Key Lab of Groundwater Resources and Environment Ministry of Education, Jilin University, Changehun 130012, China;2College of Chemistry, State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, Jilin University, Changehun 130012, Chin)

机构地区：[1]吉林大学环境与资源学院,地下水资源与环境教育部重点实验室,长春130012 [2]吉林大学化学学院,无机合成与制备化学国家重点实验室,长春130012

出　　处：《分析化学》2018年第6期883-888,共6页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(Nos.21404047,21307040); 高等学校学科创新引智计划(No.B16020)资助

摘　　要：采用电喷雾萃取电离质谱技术(Extractive electrospray ionization mass spectrometry,EESI-MS)分析水样中的有机污染物邻苯二甲酸二(2-乙基己基)酯(Di-2-ethylhexy phthalate,DEHP),系统考察了电喷雾电压、离子传输管温度、样品溶液流速及萃取剂组成对待测物信号强度的影响,优化了检测DEHP的实验条件,建立了水样中DEHP的快速质谱分析方法,并对垃圾渗滤液、城市生活污水及湖水等实际水样进行检测。结果表明,在正离子检测模式下,水样中的DEHP能够在EESI源中有效电离,生成准分子离子[M+H]^+(m/z 391.28),进行碰撞诱导解离得到二级特征碎片离子m/z 279.26,167.12,149.11。在5~1000μg/L范围内,DEHP浓度与m/z 149.11质谱峰信号强度的线性关系良好,相关系数R^2=0.9991,检出限LOD=0.21μg/L(S/N=3);水样的3个加标水平(8,80和400μg/L)的DEHP回收率为96.2%~111.2%,RSD为5.6%~11.8%。EESI-MS法检测垃圾渗滤液、城市生活污水和晏湖水中DEHP的含量分别为556.5、275.3和37.8μg/L。本方法具有无需样品预处理、分析速度快(单个样品分析时间约3 min)、操作简便、灵敏度高等优点,为邻苯二甲酸酯类物质的检测提供了一种快速质谱分析新方法。The environmental organic pollutant of di-2-ethylhexy phthalate（ DEHP） was analyzed by extractive electrospray ionization mass spectrometry（ EESI-MS）. Effect of some important experimental conditions were investigated systematically,including the electrospray voltage,temperature of ion-transport tube,sample injection rate and extractant composition. Under the optimal conditions,a method for rapid detection of DEHP in water sample was established. DEHP levels in different samples with complex matrixes were measured,including landfill leachate,urban sewage and lake water. The results showed that DEHP in water samples could be ionized by EESI source and obtained the molecule ion（ m/z 391.28） at the positive detection mode,and then CID experiment were performed to obtain the secondary fragment ions m/z 279.26,167.12 and 149. 11. The intensity of characteristic peak m/z 149. 11 possessed a good linearity with the concentration of DEHP in the range of 5-1000 μg/L with the correlation coefficient of R^2= 0.9991,and the detection limit（ LOD） of 0.21 μg/L. The recoveries of DEHP at three spiked levels（ 8,80,400 μg/L） were96.2%-111.2%,with RSDs of 5. 6%-11. 8%. With the developed EESI-MS method,the concentrations of DEHP in landfill leachate,urban sewage and Yan lake water were 556.5,275.3 and 37.8 μg/L,respectively.The EESI-MS method possessed many advantages such as no requirement of sample pretreatment,fast analysis speed（ about 3 min per sample）, simple operation and high sensitivity, thus providing a new mass spectrometric method for rapid detection of phthalate esters.

关 键 词：电喷雾萃取电离 质谱 邻苯二甲酸二(2-乙基己基)酯 环境水样 

分 类 号：O657.63[理学—分析化学] X832[理学—化学]