液相色谱-质谱法测定土壤和沉积物中的六溴十二烷  

Determination of Hexabromocyclododecane in Soils and Sediments by LC-MS

作　　者：朱明吉 孙静[1] 邓力[1] 郭志顺[1] 张芹[1] 

机构地区：[1]重庆市环境监测中心,重庆401147

出　　处：《理化检验（化学分册）》2015年第6期775-777,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：环保公益性行业科研专项(20120916)资助

摘　　要：采用液相色谱-质谱法测定土壤和沉积物中六溴十二烷的含量。样品经索氏提取器或ASE快速溶剂萃取仪，用正己烷-二氯甲烷（1＋1）混合溶剂提取，经硅胶净化柱净化。以Hypersil C18色谱柱为固定相，以水和甲醇-乙腈（8＋2）溶液为流动相进行梯度洗脱，采用电喷雾负离子源-选择反应监测模式检测。α-六溴环十二炕、伊六溴环十二炕和γ-六溴环十二炕的质量浓度的线性范围为5．0-500μg·L-1，方法的检出限（3S／N）分别为12．5，12．4，9．95ng·kg-1。应用该方法对土壤和沉积物中的六溴环十二烷进行测定，加标回收率在78．5％～111％之间，测定值的相对标准偏差（n=7）为4．1％～11％。A method of LCMS was applied for the determination of hexabromocyclododecane in soils and sediments. The sample was extracted with a mixture of n hexane and dichloromethane using. Soxhlet extractor or ASE Accelerated Solvent Extractor, and then purified on silica gel column. The Hypersil C18 column was used as stationary phase and the mixture of water and methnol-acetonitrile was used as mobile phase for gradient elution. ESI and SRM were adopted in MS/MS detection. The linearity ranges for a-hexabromocyclododecan β- hexabromocyclododecane and y-hexabromocyclododecane were all within 5.0--500 μg · L-1, with detection limits （3S/N） of 12.5, 12. 4 and 9. 95 ng ·kg-1 , respectively. The method was used to measure soils and sediments samples, recovery rate measured by standard addition method was in the range of 78. 5%--111% with RSD＇s （n= 7） in the range of 4.1%--11%.

关 键 词：液相色谱-质谱法 六溴环十二烷 土壤 沉积物 

分 类 号：O657.63[理学—分析化学]