分散液液微萃取-上浮溶剂固化/高效液相色谱法测定沉积物中的十溴联苯醚  

Dispersive Liquid-Liquid Microextraction Based on Solidification of Floating Organic Drop with High Performance Liquid Chromatography for Determination of Decabrominated Diphenyl Ether in Surficial Sediments

作　　者：翦英红[1,2] 胡艳[3] 王婷[3] 刘建林[3] 张琛[3] 李鱼[3,1] 

机构地区：[1]吉林大学环境与资源学院,长春130012 [2]吉林化工学院环境与生物工程学院,吉林132022 [3]华北电力大学能源与环境中心,北京102206

出　　处：《分析化学》2010年第1期62-66,共5页Chinese Journal of Analytical Chemistry

基　　金：国家“973”计划项目(NO.2004CB418501)资助

摘　　要：建立了沉积物中痕量十溴联苯醚的分散液液微萃取-上浮溶剂固化-高效液相色谱-紫外法(DLLME-SFO-HPLC-UV)。以正交试验数据为训练样本,采用BP(Back propagation)神经网络模型优化了分散液液微萃取-上浮溶剂固化条件:分散剂为1.00mL甲醇、萃取剂为35.0μL十二醇、NaCl质量浓度为10.00%、萃取时间10min和pH=5,其萃取率(ER)可达62.22%。方法的线性范围为3.5～1400ng/g(r=0.9960),检出限(LOD)和定量限(LOQ)分别为2.3pg/g(S/N=2)和5.6pg/g(S/N=5),实际样品的加标回收率为97.7%～104.2%。本方法集萃取、富集、分离步骤于一体,简化了沉积物中十溴联苯醚的前处理过程。A method for the determination of decabrominated diphenyl ether（decaBDE） in sediment samples at trace level using dispersive liquid-liquid microextraction based on the solidification of floating organic drop （DLLME-SFO） and high performance liquid chromatography-ultraviolet detector（HPLC-UV） has developed.Based on the data of interactive orthogonal array design,the optimization experimental conditions were obtained with BP artificial neural network model：1.00 mL methanol as dispersive solvent,35.0 μL dodecanol as extractive solvent,10.00% NaCl,pH 5,and extraction in 10 min.The extraction recovery（ER） was 62.22% at the extraction conditions.The proposed method exhibited a wide linear range（3.5-1400 ng/g） with R2=0.9921.The limit of detection（LOD） and the limit of quantification（LOQ） of this method were 2.3 pg/g（S/N=2） and 5.6 pg/g（S/N=5）,respectively.The recoveries of real samples at different spiking levels of decaBDE were 104.2%,98.4% and 97.7%,respectively.Extraction,concentration and separation procedures for decaBDE from the sediment sample were carried out by one step,and hence,the process of DLLME-SFO for decaBDE was shortened.

关 键 词：分散液液微萃取 上浮溶剂固化 高效液相色谱-紫外法 沉积物 十溴联苯醚 多层前馈神经网络 

分 类 号：X830.2[环境科学与工程—环境工程]