Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran.
Anal Chim Acta. 2013 Aug 20;792:59-65. doi: 10.1016/j.aca.2013.07.020. Epub 2013 Jul 15.
A novel high-throughput device based on 96-micro-solid phase extraction (96-μ-SPE) system was constructed for multiresidue determination of nine pesticides in aquatic samples. The extraction procedure was performed on a commercially available 96-well plate system. The extraction module consisted of 96 pieces of 1cm×3cm of cylindrically shaped stainless steel meshes. The prepared meshes were fixed in a home-made polytetrafluoroethylene-based constructed ninety-six holes block for possible simultaneous immersion of meshes into the center of individual wells. Dodecyl methacrylate and ethylene glycol dimethacrylate was copolymerized as a monolithic polymer and placed in the cylindrically shaped stainless steel meshes as extracting medium. A volume of 1mL of the aquatic sample was transferred into the 96-well plate and the 96-μ-SPE device was applied for the extraction of the selected pesticides. Subsequently, the extracted analytes were analyzed by gas chromatography-mass spectrometry. Influential parameters such as polymer synthesis conditions, sorbent-to-sorbent reproducibility, ionic strength and extraction time were optimized. Intra and inter-sorbent reproducibility on 96-μ-SPE device were evaluated and results revealed that extraction yields are rather similar. Limits of detection were below 4μg L(-1) and the coefficient of determination was satisfactory (r(2)>0.99) for all the studied analytes. The developed method was successfully applied to the extraction and determination of the selected pesticides in surface water samples.
一种新型高通量基于 96 微固相萃取(96-μ-SPE)系统的设备被构建用于在水样中多残留测定九种农药。萃取程序在市售的 96 孔板系统上进行。萃取模块由 96 个 1cm×3cm 的圆柱形不锈钢网格组成。将准备好的网格固定在自制的聚四氟乙烯构建的 96 孔块中,以便将网格同时浸入各个孔的中心。十二烷基甲基丙烯酸酯和乙二醇二甲基丙烯酸酯共聚作为整体聚合物并放置在圆柱形不锈钢网格中作为萃取介质。将 1mL 水样转移到 96 孔板中,并应用 96-μ-SPE 装置提取选定的农药。随后,通过气相色谱-质谱法分析提取的分析物。优化了聚合物合成条件、固定相之间的重现性、离子强度和萃取时间等影响参数。在 96-μ-SPE 装置上评估了内和固定相之间的重现性,结果表明萃取产率非常相似。所有研究的分析物的检测限均低于 4μg L(-1),且决定系数令人满意(r(2)>0.99)。所开发的方法成功地应用于地表水样品中选定农药的提取和测定。