Rodil Rosario, Moeder Monika
Department of Analytical Chemistry, University of A Coruña, Campus da Zapateira, 15071 A Coruña, Spain.
J Chromatogr A. 2008 Jan 18;1178(1-2):9-16. doi: 10.1016/j.chroma.2007.11.051. Epub 2007 Nov 22.
Stir bar sorptive extraction (SBSE) in combination with thermodesorption-gas chromatography-mass spectrometry (TD-GC-MS) was applied for the determination of eight insect repellents and synergists in water samples. The stir bar coated with polydimethylsiloxane (PDMS) was added to 20 mL of water sample with 4 g NaCl and stirred at 1000 rpm for 180 min. Then, the stir bar was subjected to TD-GC-MS. SBSE parameters (ionic strength, presence of organic solvent and time) were optimised. Blank contamination and carryover problems were also studied. The method affords detection limits between 0.5 and 30 ng/L, except for dimethyl phthalate (DMP) (150 ng/L) due to blank contamination problems. It shows good linearity with correlation coefficients over 0.997 and reproducibility (RSD) below 20%. The extraction efficiencies were between 29% for DMP and 80% for di-n-propyl isocinchomeronate (R-326). The feasibility of the method was tested by analysing real samples such as lake water, river water and wastewater.
搅拌棒吸附萃取（SBSE）结合热脱附-气相色谱-质谱联用（TD-GC-MS）用于测定水样中的八种驱虫剂和增效剂。将涂有聚二甲基硅氧烷（PDMS）的搅拌棒加入到含有4 g氯化钠的20 mL水样中，以1000 rpm搅拌180分钟。然后，将搅拌棒进行热脱附-气相色谱-质谱分析。对SBSE参数（离子强度、有机溶剂的存在和时间）进行了优化。还研究了空白污染和残留问题。该方法的检测限在0.5至30 ng/L之间，但由于空白污染问题，邻苯二甲酸二甲酯（DMP）的检测限为150 ng/L。它具有良好的线性，相关系数超过0.997，重现性（相对标准偏差，RSD）低于20%。萃取效率在DMP的29%至异壬酸二正丙酯（R-326）的80%之间。通过分析湖水、河水和废水等实际样品测试了该方法的可行性。
