固相微萃取-气相色谱质谱法联用测定水体中痕量多环麝香类化合物  

Optimization of solid-phase microextraction for the gas chromatographic-mass spectrometric determination of polycyclic musk compounds in water

作　　者：韩潇[1] 陈东辉[2] 黄满红[1] 

机构地区：[1]东华大学环境科学与工程学院,上海201620 [2]上海应用技术学院化学与环境工程学院,上海200235

出　　处：《分析试验室》2012年第4期59-63,共5页Chinese Journal of Analysis Laboratory

基　　金：上海科委项目(09230500200);教育部博士点基金项目(20090075120007);国家自然科学基金(21007010);中央高校基本科研基金(2011D11309)资助

摘　　要：采用固相微萃取-气相色谱质谱法联用测定了水体中痕量多环麝香类化合物。对固相微萃取条件和解析条件进行了优化,确定了微萃取条件为:选用65μmPDMS-DVB萃取头、顶空萃取模式(HS),在800 r/min,60℃条件下,萃取45 min;萃取过程中保持pH 7并且不加入NaCl;解析条件为:解析时间为3 min,插入GC深度为4 cm,进样口温度为250℃。方法的检测限为0.29～0.37 ng/L,线性范围5～1000ng/L,相对标准偏差1.5%～2.2%。对实际污水厂不同类型的水样使用优化后的实验条件进行了验证试验,目标化合物的回收率在82.5%～92.8%之间,表明优化后的试验条件适用于实际水体中痕量多环麝香类化合物的分析测定。A solid-phase microextraction method for determining trace levels of polycyclic musk in water had been developed.Compared with the different parameters affecting the extraction process,the most effective extraction were achieved by optimized conditions which were 65μmPDMS-DVB,headspace extraction mode,stirrering at 800 r/min,PH 7,extraction times of 45 min at 60℃ with no need of NaCl.And injection temperature of 25 ℃,4cm of injection depth with 3min desorption time for the desorption conditions.The detection limits were between 0.29 and 0.37 ng/L and the relative standard deviations were 1.5%~2.2%.Good spiked recoveries ranging from 82.5% to 92.8% were reached from real samples which were taken from two urban treatment plants which in dicate that the optimized method can be applicable to the determination of trace polycylic musk in real water samples.

关 键 词：固相微萃取 水体分析 多环麝香 

分 类 号：O657.63[理学—分析化学]