Van Hoeck Els, David Frank, Sandra Pat
Department of Organic Chemistry, Ghent University, Krijgslaan 281, S4-bis, B-9000 Gent, Belgium.
J Chromatogr A. 2007 Jul 20;1157(1-2):1-9. doi: 10.1016/j.chroma.2007.04.036. Epub 2007 Apr 20.
Stir bar sorptive extraction (SBSE) was applied to the enrichment of pyrethroids in water samples. Analysis was done by retention time-locked GC/MS in selected ion-monitoring (SIM) mode using trans-permethrin-d(6) as internal standard. Thermal desorption (TD) was performed in a classical split/splitless inlet equipped with a flip-top sealing system and in a dedicated thermal desorption unit. These two thermal desorption methods were compared to liquid desorption with ethyl acetate. Sensitivity was the highest for thermal desorption in the dedicated system and the lowest for liquid desorption even at injection volumes of 10 microL. The SBSE-TD-GC/MS method is able to determine pyrethroids at ultra-trace level (<1 ng/L) with RSD% smaller than 15 (n=6).
搅拌棒吸附萃取（SBSE）用于富集水样中的拟除虫菊酯。采用反式氯菊酯 - d(6)作为内标，通过保留时间锁定气相色谱/质谱联用仪在选择离子监测（SIM）模式下进行分析。热脱附（TD）在配备翻盖密封系统的经典分流/不分流进样口中以及专用热脱附单元中进行。将这两种热脱附方法与用乙酸乙酯进行的液体脱附进行了比较。在专用系统中热脱附的灵敏度最高，即使进样体积为10微升时，液体脱附的灵敏度也是最低的。SBSE - TD - GC/MS方法能够测定超痕量水平（<1 ng/L）的拟除虫菊酯，相对标准偏差（RSD%）小于15（n = 6）。
