GC-NCI-MS法测定底泥中类二英多氯联苯  

Determination of Dioxin-like PCBs in Sediment by Gas Chromatography/Negative Chemical Ionization/Mass Spectrometry

作　　者：马召辉[1] 金军[1] 王英[1] 亓学奎[1] 丁问微[1] 姜霞[2] 吴小兵[1] 

机构地区：[1]中央民族大学生命与环境科学学院,北京100081 [2]中国环境科学研究院,北京100012

出　　处：《环境科学与技术》2011年第10期123-126,共4页Environmental Science & Technology

基　　金：高等学校学科创新引智计划(B08044);国家大学生创新性实验计划(NMOE200911026);北京高等学校化学实验教学示范中心建设项目(2008);国家重大科技专项资助(2008ZX07101-010-04-1)

摘　　要：建立了气相色谱/负化学负离源/质谱（GC-NCI-MS）法测定底泥样品中世界卫生组织（WHO）推荐的12种类二英多氯联苯。底泥样品采用索氏提取,酸碱复合硅胶柱净化,选择离子扫描监测,同位素稀释内标法定量。比较PCBs各单体在负化学负离源（NCI）和电子轰击电离源（EI）条件下的灵敏度,发现PCBs各单体在NCI条件下的灵敏度是EI条件下的21~100倍。用GC-NCI-MS法分析类二英多氯联苯,仪器检出限为0.1 pg,方法检出限为1~1.2 pg/g,3个平行基质土样品加标回收率为84%~119%。应用建立的方法对太湖底泥中12种类二英和PCB170、PCB180进行测定,结果表明,底泥样品中∑14PCBs含量为7.5~470 pg/g（干重）,平均值108 pg/g（干重）。PCBs单体浓度范围为n.d.~155 pg/g干重,在检测的14种同族体中PCB118是主要的同族体,其次是PCB77、PCB105。A gas chromatography/negative chemical ionization/mass spectrometry（GC-NCI-MS）method was developed for determination of 12 types of dioxin-like PCBs which recommended by WHO.Sediment samples were extracted by Soxhlet apparatus,and cleaned with acid-base composite silica gel column,selected ion scan and quantified by isotope dilution method.Results showed that the sensitivity under NCI source measuring dioxin-like PCBs were 21~100 times higher than EI source.Under the method,the study obtained a lower instrument detection limit of 0.1 pg,the recovery of spiking three parallel matrix soil samples ranged from 84%~119%.The established method was used for determination of dioxin-like PCBs,PCB170 and PCB180 in sediment samples of Taihu Lake,results indicated that the concentration of PCBs were from 7.5 to 470 pg/g（dry weight）and average concentration was 108 pg/g（dry weight）.Individual PCBs congeners concentration was from n.d.~155 pg/g（dry weight）.Among these 14 congeners,PCB118 was the main congeners,followed by PCB77 and PCB105.

关 键 词：类二噁英多氯联苯 气相色谱/负化学离子源/质谱 底泥 

分 类 号：X830.2[环境科学与工程—环境工程]