搅拌棒萃取-热解吸气相色谱法测定水中倍半芥子气  

Determination of Sesquimustard in Water Using Stir Bar Sorptive Extraction-Thermal Desorption-Gas Chromatography

作　　者：曲刚莲[1] 刘国宏[1] 马果花[1] 李芬润[1] 

机构地区：[1]防化指挥工程学院三系,北京102205

出　　处：《分析化学》2007年第8期1215-1217,共3页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金资助项目(No20605027)

摘　　要：建立了一种以SBSE萃取与热解吸-气相色谱-火焰光度法联用技术为基础的测定水中倍半芥子气的方法。对比了SBSE和固相微萃取(SPME)对水中的倍半芥子气的萃取回收率,实验结果表明,SBSE对倍半芥子气的萃取率在22.47%～22.60%之间,SPME对倍半芥子气的萃取率为0.4%。研究了萃取时间、解吸附时间、样品溶液pH值、萃取温度对萃取回收率的影响,选择萃取时间为20min、一级解吸时间为10min、二级解吸时间为4min、样品溶液pH值为7.0、萃取温度为25℃。检测倍半芥子气的线性范围为0.462～23.1μg/L,最低检出限为0.0924μg/L(S/N=3)。该方法已成功应用于河水的检测。A method based on stir bar sorptive extraction （SBSE） hyphenated with gas chromatography-flame photometric detector （GC-FPD） was established for the determination of sesquimustard in water. The extrac- tion recoveries of sesquimustard in water were compared between SBSE and solid-phase microextraction （SPME）. The experimental results showed that the recovery of sesquimustard using SBSE was 22.47% - 22. 60% and 0.4% using SPME. The effects of extraction time, desorption time, pH value and extraction temperature on the extraction recovery were investigated. The extraction time was 20 min ; the primary desorp- tion time was 10 min, and the secondary desorption time was 4 min ; the pH value was 7.0 ; the extraction temperature was 25℃. The linear range for sesquimustard was 0. 462 -23.1 μg/L. The detection limit （3s） for sesquimustard was 0. 0924 μg/L. The method has been applied to the analysis of canal water.

关 键 词：搅拌棒萃取 倍半芥子气 热解吸 气相色谱 

分 类 号：O661.1[理学—分析化学] O657.71[理学—化学]