加速溶剂萃取-硅胶柱净化-碱性氧化铝柱分离-气相色谱三重四极杆质谱法测定土壤中的二英类化合物  

Determination of Dioxin-like Compounds in Soil by Accelerated Solvent Extraction-Silica Gel Column Cleanup-Basic Alumina Column Separation Coupled with Gas ChromatographyTriple Quadrupole Mass Spectrometry

作　　者：邬静[1] 胡吉成[1,2] 马玉龙[1] 王世杰[1] 王英[1,2] 金军[1,2] 

机构地区：[1]中央民族大学生命与环境科学学院,北京100081 [2]北京市食品环境与健康工程中心,北京100081

出　　处：《分析化学》2017年第6期799-808,共10页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.21407185);中央高校基本科研业务费专项资金(Nos.2017MDYL31;2015MDTD23C);高等学校学科创新引智计划(No.B08044);国家大学生创新训练计划(No.GCCX2016110042)资助项目~~

摘　　要：建立了加速溶剂萃取(ASE),酸性硅胶柱、复合硅胶柱及碱性氧化铝柱纯化分离,气相色谱-三重四极杆质谱测定土壤中二英/呋喃(PCDD/Fs)、多氯联苯(PCBs)、多氯萘(PCNs)的分析方法。选用正己烷-二氯甲烷(50∶50,V/V)作为ASE的提取溶剂,设定提取温度为120℃,加标回收实验表明本方法可行。用100 m L正己烷-二氯甲烷(95∶5,V/V)及50 m L正己烷-二氯甲烷(50∶50,V/V)依次淋洗碱性氧化铝柱,得到组分A(PCBs及PCNs)与组分B(PCDD/Fs),实现了PCDD/Fs与另外两种化合物的分离,排除了同系物间及其它杂质的干扰。使用同位素稀释-气相色谱三重四极杆质谱法(GC-MS/MS),在选择反应监测(Selected reaction monitoring,SRM)模式下测定PCDD/Fs、PCBs和PCNs,3种化合物的仪器检出限(LOD)范围分别为0.04~0.25μg/L,0.10~0.20μg/L和0.01~0.05μg/L,目标物平均相对响应因子(RRF)的相对标准偏差(RSD)均小于13%。基质土加标实验中,3种化合物13C标记的同位素内标回收率的范围分别为50%~95%,51%~103%,49%~74%。实际样品的分析结果表明,PCDD/Fs、PCBs及PCNs在土壤样品中的总含量范围分别为16.1~1148 pg/g、6.6~152.6 pg/g及10.9~99.5 pg/g,且样品测定结果与高分辨质谱测定结果相吻合。A method for determination of PCDD/Fs, PCBs and PCNs in soil sample was developed by using accelerated solvent extraction （ASE）-silica gel column cleanup-basic alumina column separation coupled with GC-MS/MS. The sample was extracted by ASE with Hexane-methylene chloride （Hex- DCM,5 0 ：50, V /V） at120℃ .The basic alumina column was used to separate PCDD/Fs, PCBs and PCNs. The extracts were eluted with Hex-DCM （95 ： 5, V/V ） to obtain PCBs and PCNs, followed by Hex-DCM （50：5 0 , V/V） to obtain PCDD/Fs. The limits of detection （LOD） were in the range of 0. 04-0. 25 μg /L ,0.10 - 0.20μg /L and 0.01-0.05 μg/L for PCDD/Fs, PCBs, PCNs, respectively. The relative standard deviations （RSDs） of average relative response factors （RRF） were below 13%. The recoveries of 13C-labeled internal standards of the three classes of analytes were 50% -95% , 51%-103% and 49% -74% , respectively. Concentrations of [PCDD/Fs,∑PCBs and ∑PCNs in soil samples were 16. 1-1148 pg/g, 6.6-152.6 pg/g and 10. 9-99.5 pg/g, respectively. The results were consistent with that of high resolution mass spectrometer.

关 键 词：二英/呋喃 多氯联苯 多氯萘 前处理方法 三重四极杆质谱 

分 类 号：O657.63[理学—分析化学] X833[理学—化学]