加速溶剂萃取-气相色谱串联质谱法检测沉积物中痕量增塑剂  

Determination of Phthalate Esters in Sediment Using Accelerated Solvent Extraction and Gas Chromatography-Mass Spectrometry

作　　者：邵海洋[1] 徐刚[2] 吴明红[1] 唐亮[1] 刘宁[1] 裘文慧[1] 

机构地区：[1]上海大学环境与化学工程学院,上海200444 [2]上海大学射线应用研究所,上海200444

出　　处：《分析化学》2013年第9期1315-1321,共7页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(Nos.11025526;41073073;11175112;41173120)资助项目

摘　　要：研究了加速溶剂萃取(ASE)对沉积物中邻苯二甲酸酯类(PAEs)物质的提取效果,建立了快速溶剂萃取/气相色谱-质谱联用(GC/MS)检测沉积物中16种邻苯二甲酸酯类物质的方法。用正己烷和二氯甲烷混合溶剂作为提取溶剂,加速溶剂萃取法萃取沉积物中16种PAEs,再用Florisil层析柱净化,最后用GC/MS对净化后提取液中的PAEs进行定量分析。结果表明:当萃取剂为二氯甲烷-正己烷(1∶1,V/V),萃取温度为80℃时,萃取效率最高,16种PAEs的回收率稳定在81.2%～128.5%之间,相关系数≥0.99,检出限为0.12～0.98 ng/g,相对标准偏差为1.1%～10.8%。加速溶剂萃取法与传统索氏提取法相比,既提高了萃取效率同时又减少了有机萃取溶剂的用量。在检测实际样品时,同时加入3种内标指示剂对方法的性能进行了验证,3种内标的回收率分别为106.0%±18.8%,87.4%±10.8%和81.4%±14.5%,样品中16种PAEs的检出率为100%。前处理方法处理简单,定性与定量分析准确可靠。The extraction efficiency of accelerated solvent extraction（ASE） was studied for Phthalate Esters in sediment and compared with that of Soxhlet.A method has been developed for the detection of 16 phthalate esters（PAEs） in sediment samples by ASE and gas chromatography-mass spectrometry（GC/MS）.The samples were extracted using ASE with dichloromethane-hexane mixture,and then the extracts were purified by Florisil column.After cleanup,the extracts were analyzed by GC/MS in SIM mode,using characteristic ions for quantification.The results showed that dichloromethane-hexane mixture displayed the best extraction performance among the three employed solvents,80 ℃ was the best extraction temperature.In comparison with Soxhlet extraction method,not only the efficiency of ASE was generally better than Soxhlet,but reduced solvent consumption.The average recoveries were from 81.2% to 128.5%,the correlation coefficient was more than 0.99,and the limits of detection（LOD） of all the compounds were 0.12-0.98 ng/g with RSDs less than 10.8%.

关 键 词：邻苯二甲酸酯 加速溶剂萃取 气相色谱质谱 沉积物 

分 类 号：X832[环境科学与工程—环境工程] O657.63[理学—分析化学]