Rodil Rosario, Moeder Monika
Department of Analytical Chemistry, University of A Coruña, Campus da Zapateira, 15071-A Coruña, Spain.
J Chromatogr A. 2008 Feb 1;1179(2):81-8. doi: 10.1016/j.chroma.2007.11.090. Epub 2007 Dec 4.
Stir bar sorptive extraction (SBSE) in combination with thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS) was applied for the determination of 9 UV filters in water samples. The stir bar coated with polydimethylsiloxane (PDMS) was added to 20 mL of water sample at pH 2 (10% MeOH) and stirred at 1000 rpm for 180 min. Then, the stir bar was subjected to TD-GC-MS. The desorption conditions (desorption temperature and desorption time) and SBSE parameters (ionic strength, pH, presence of organic solvent and time) were optimised using a full factorial design and a Box-Behnken design, respectively. The method shows good linearity (correlation coefficients >0.994) and reproducibility (RSD<16%). The extraction efficiencies were above 63% for all the compounds. Detection limits were between 0.2 and 63 ng/L. The developed method offers the ability to detect several UV filters at ultra-low concentration levels with only 20 mL of sample volume. The effectiveness of the method was tested by analysing real samples such as lake water, river water and treated wastewater. The application of the method allowed reporting the levels of UV filters in environmental water samples.
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9种紫外线过滤剂。将涂有聚二甲基硅氧烷(PDMS)的搅拌棒加入到20 mL pH为2(含10%甲醇)的水样中,以1000 rpm搅拌180分钟。然后,将搅拌棒进行TD-GC-MS分析。分别采用全因子设计和Box-Behnken设计对脱附条件(脱附温度和脱附时间)和SBSE参数(离子强度、pH、有机溶剂的存在和时间)进行了优化。该方法具有良好的线性(相关系数>0.994)和重现性(RSD<16%)。所有化合物的萃取效率均高于63%。检测限在0.2至63 ng/L之间。所开发的方法能够仅用20 mL样品体积在超低浓度水平下检测多种紫外线过滤剂。通过分析湖水、河水和处理后的废水等实际样品对该方法的有效性进行了测试。该方法的应用能够报告环境水样中紫外线过滤剂的含量。