Celeiro Maria, Facorro Rocio, Dagnac Thierry, Llompart Maria
Laboratory of Research and Development of Analytical Solutions (LIDSA), Department of Analytical Chemistry, Nutrition and Food Science, Faculty of Chemistry, E-15782, Campus Vida, Universidade de Santiago de Compostela, Santiago de Compostela, Spain.
Laboratory of Research and Development of Analytical Solutions (LIDSA), Department of Analytical Chemistry, Nutrition and Food Science, Faculty of Chemistry, E-15782, Campus Vida, Universidade de Santiago de Compostela, Santiago de Compostela, Spain; Agronomic and Agrarian Research Centre (INGACAL-CIAM), Unit of Organic Contaminants, Apartado 10, 15080, A Coruña, Spain.
Anal Chim Acta. 2018 Aug 22;1020:51-61. doi: 10.1016/j.aca.2018.03.014. Epub 2018 Mar 20.
A solvent-free method based on solid-phase microextraction (SPME) followed by gas chromatography-tandem mass spectrometry (GC-MS/MS) has been developed for the simultaneous determination of eleven fungicides at trace levels in different types of waters. Several experimental SPME parameters such as temperature, fibre coating, and SPME mode, were optimized in order to obtain the highest extraction efficiency. Under the optimal conditions, 100 °C, polyacrilate fibre (PA) and direct-immersion mode, the method was validated showing good linearity, repeatability and reproducibility. Recovery studies were carried out in four different real water matrices and at three concentration levels (20, 200 and 2000 ng L), with overall recovery values between 92 and 104% and relative standard deviations (RSD) about 10%. Limits of detection (LODs) at the low ng L were obtained. The method demonstrated its suitability for the determination of fungicides in real water samples using external calibration for quantification purposes as well as for photodegradation studies at low concentration levels.
已开发出一种基于固相微萃取(SPME)并结合气相色谱-串联质谱(GC-MS/MS)的无溶剂方法,用于同时测定不同类型水体中痕量水平的11种杀菌剂。对诸如温度、纤维涂层和SPME模式等几个实验性SPME参数进行了优化,以获得最高的萃取效率。在最佳条件下,即100°C、聚丙烯酸酯纤维(PA)和直接浸入模式下,该方法经验证具有良好的线性、重复性和再现性。在四种不同的实际水样基质中以及三个浓度水平(20、200和2000 ng/L)下进行了回收率研究,总体回收率在92%至104%之间,相对标准偏差(RSD)约为10%。获得了低ng/L水平的检测限(LOD)。该方法证明了其适用于使用外标法进行定量的实际水样中杀菌剂的测定,以及低浓度水平下的光降解研究。