超高效液相色谱-电喷雾离子源-串联三重四极质谱分析土壤中六溴环十二烷  

Determination of Hexabromocyclododecane Diastereomers in Soil by Ultra Performance Liquid Chromatography-Electrospray Ion Source/Tandem Mass Spectrometry

作　　者：金军[1] 杨从巧[1] 王英[1] 刘安明 

机构地区：[1]中央民族大学生命与环境科学学院,北京100081 [2]滨海人民医院,潍坊262737

出　　处：《分析化学》2009年第4期585-588,共4页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.20507023);中央民族大学985工程(No.CUN985-3-3)资助项目

摘　　要：建立了加速溶剂萃取-超高效液相色谱-电喷雾离子源-串联三重四极质谱(ASE-UPLC-ESI-MS/MS)分析环境土壤样品中六溴环十二烷(HBCD,C12H18Br6)3个主要异构体α-、β-、γ-HBCD的方法。土壤样品用正己烷/丙酮(3∶1,V/V)萃取,采用由下往上填充6g活性硅胶、3g44%酸性硅胶(w/w)、3g无水硫酸钠的复合硅胶柱富集纯化,内标法定量。3个平行基质土样本加标54ngΣHBCD,ΣHBCD回收率为(104.6±3.7)%。应用建立的方法对HBCD生产工厂周围环境土壤样品中α-、β-、γ-HBCD进行了测定,土壤样品中ΣHBCD含量为2.8～144.5ng/g干重。γ-HBCD是土壤样品中主要HBCD异构体(73.7±4.7)%;其次为α-HBCD(14.6±3.4)%;β-HBCD含量最低(11.7±1.7)%。A new method dedicated to trace level measurement of α-,β- and γ-HBCD （ hexabromoccyelodecane） diastereomers （C12H18Br6 ）in soil samples by accelerated solvent extraction-ultra performance liquid chromatography-electrospray ion source-triple quadrupole mass spectrometry （ASE-UPLC-ESI-MS/MS） has been developed. Soil samples were extracted with 3：1 hexane/acetone （v/v） , and was further cleaned with one muttilayer silica column （ 15 mm i. d. ） filled from the bottom with 6 g of activated silica, 3 g of H2SO4/ silica 44% （w/w） and 3 g dried Na2SO4. Quantification of the α-,β- and γ-HBCD diastereomers in samples were determined by the internal standard method. The recovery of triplicate spiked blank soil samples was （ 104.6 ± 3.7 ） % for the spiked level of 54 ng ∑HBCD. The concentrations of ∑HBCD in soil samples collected near a HBCD manufactory ranged from 2.8 to 144.5 ng/g（ dry weight）. The diastereomer profile of HBCD in the soil samples was dominated by γ-HBCD（73.7 ±4.7）% and followed by α- HBCD（14.6 ±3.4）% and β-HBCD（11. 7 ±1.7）%.

关 键 词：六溴环十二烷异构体 超高效液相色谱/电喷雾/串联质谱 土壤 加速溶剂萃取 

分 类 号：X833[环境科学与工程—环境工程]