超声辅助离子液体微萃取-液相色谱-串联质谱法测水中六溴环十二烷  

Rapid Determination of Hexabromocyclododecane Diastereomers in Water Samples by Ultrasound-Assisted Ionic Liquid Microextraction Coupled with LC-MS-MS

作　　者：姚宇翔[1,2] 苑金鹏[2] 吕海波[1] 钱晓迪[1] 孙友敏[1] 

机构地区：[1]山东建筑大学市政与环境工程学院,山东济南250101 [2]山东省分析测试中心,山东济南250014

出　　处：《中国环境监测》2016年第2期95-99,共5页Environmental Monitoring in China

基　　金：国家自然科学基金(41173092);济南市科技局高校院所自主创新计划项目(201102046)

摘　　要：建立了超声辅助离子液体液-液微萃取（USA-IL-DLLME）结合液相色谱-串联质谱测定水中六溴环十二烷3种异构体（α-HBCD、β-HBCD、γ-HBCD）的分析方法。实验中分别考察了离子液体萃取剂的种类及体积、超声时间、样品p H及盐浓度等因素的影响。在最佳条件下,HBCDs 3种异构体在0.5-100μg/L质量浓度条件下有较好的线性关系,相关系数大于0.998,最低检出限分别为156.4、84.6、85.5 ng/L,测定下限分别为0.626、0.339、0.342μg/L。相对标准偏差（n=5）为5.3%-9.7%。采用该方法对实际环境水样进行了检测与加标回收实验,在1、20μg/L 2个添加水平下,加标回收率为71%-102%。方法具有简单快速、有机溶剂用量少、绿色环保的特点。A rapid analysis method,ultrasound-assisted ionic liquid dispersive liquid liquid microextraction（ USA-IL-DLLME）coupled with LC-MS-MS,has been developed for the determination of hexabromocyclododecane diastereomers（ α-HBCD,β-HBCD,γ-HBCD） in environmental water samples. The factors influencing extraction efficiencies,including kinds and volume of ionic liquid,ultrasonic time,the sample p H and salt concentration,were investigated and optimized. Under the optimum conditions,the calibration graph of the proposed method was line in the range of 0. 5-100 μg / L and the correlation coefficient is greater than 0. 998. The limit of detection was 156. 4,84. 6,85. 5 ng / L and the limit of quantification was 0. 626,0. 339,0. 342 μg / L and the precisions were 5. 3%-9. 7%. The method was applied to analyze the environmental water samples and the spike recoveries at the levels of 1,20 μg / L were at about 71% to 102%. The results indicated that the proposed method was simple,quick and green alternative for the analysis of pollutants in environmental water samples.

关 键 词：USA-IL-DLLME 液相色谱-串联质谱 六溴环十二烷 

分 类 号：X832.02[环境科学与工程—环境工程]