电子垃圾污染地区生物样品中痕量多溴二苯醚的检测  

Quantification of Trace Polybrominated Diphenyl Ether in Biota Samples from an Electronic Waste Recycling Area

作　　者：梁淑轩[1] 赵茜[1] 杨中军 

机构地区：[1]河北大学化学与环境科学学院,河北保定071002 [2]南阳红宇机电有限公司,河南南阳474675

出　　处：《河北大学学报（自然科学版）》2009年第5期511-517,共7页Journal of Hebei University(Natural Science Edition)

基　　金：国家自然科学基金重点资助项目(20437020)

摘　　要：建立了气相色谱负化学电离质谱法（GC/NCI-MS）同时测定环境生物样品中一至十溴二苯醚中的42种同类物的方法.样品经过预处理后用双溶剂混合液提取,多层硅胶柱净化,浓缩后进行GC/NCI-MS测定.具有严格的质量控制和质量保证分析步骤,初始精密度实验和实验中的精密度实验的相对标准偏差（RSD）〈15%,PBDEs的仪器检出限为0.22~1.99 pg.此方法测定标准参考物质WMF-01（鱼粉）中PB-DEs,得到了满意的结果,方法简便,净化效果好,费用低.将该方法应用于电子垃圾拆解地区的生物样品中华圆田螺和泽蛙中多溴二苯醚的实际检测,多溴二苯醚质量分数最高达到25 ng/g.A gas chromatography-negative chemical ionization mass spectrometry（GC/NCI-MS） method has been established for the analysis of environmental biota samples into forty-two congeners containing mono-to deca-brominated diphenyl ethers,respectively.The samples were extracted by mixed solvent,cleaned up with multi-layer silica gel column,and then analyzed by proposed GC/NCI-MS method.Method quality control and instrumental quality control were carried out.The relative standard deviation was lower than 15% for initial precision and recovery and ongoing precision and recovery.The limits of detection were from 0.22 to 1.99 pg for EO-5278.The developed method has also been successfully applied to the determination of PBDEs in WMF-01（standard reference material,fish powder）.The method was applied to determine trace PBDEs in the mudsnail（Cipangopaludina cahayensis） and frog（Rana limnocharis） samples that were collected in heavily e-wastes polluted area,and the mass fraction of PBDEs congeners reached 25 ng/g.Compared with high resolution gas chromatography-mass spectrometry,the results indicated that the proposed method was easier,better purification effect,low-cost and suitable for wider application to analyze the PBDEs in environmental biota samples.

关 键 词：气相色谱负化学电离源质谱法 多溴二苯醚 同时测定 

分 类 号：O656.31[理学—分析化学]