Department of Chemistry, Science Faculty, Ege University, Bornova, İzmir, Turkey.
J Sep Sci. 2013 Oct;36(19):3234-41. doi: 10.1002/jssc.201300633. Epub 2013 Aug 29.
A robust solid-phase microextraction fiber was fabricated by electropolymerization of thiophene on a stainless steel wire. This fiber was applied for the determination of endocrine-disruptor pesticides, namely, chlorpyrifos, penconazole, procymidone, bromopropylate, and λ-cyhalothrin in well waters by a headspace solid-phase microextraction procedure. Operational parameters, namely, pH, sample volume, adsorption temperature and time, desorption temperature, stirring rate, and salt amount were optimized as 7.0, 8 mL, 70°C and 20 min, 250°C, 600 rpm, and 0.3 g/mL, respectively. The separation power of GC was coupled with the excellent sensitivity of the developed fiber enabling us to determine pesticide mixtures simultaneously in a ng/mL range. The LOD was in the range of 0.02-0.64 ng/mL. The method was successfully applied for the selective and sensitive determination of target pesticides in well water samples with acceptable recovery values (92-110%). The polythiophene fiber gives satisfactory results compared with commercial fibers. Commonly used pesticides with different polarities were chosen as representative compounds to search the applicability of the fiber for well water analysis collected from vineyards.
采用电化学聚合噻吩的方法在不锈钢丝上制备了一种坚固的固相微萃取纤维。该纤维应用于顶空固相微萃取程序,测定井水 中内分泌干扰农药,即氯吡硫磷、丙环唑、菌核净、溴丙酰和 λ-氯氟氰菊酯。优化了操作参数,即 pH 值、样品体积、吸附温度和时间、解吸温度、搅拌速度和盐量分别为 7.0、8 mL、70°C 和 20 min、250°C、600 rpm 和 0.3 g/mL。GC 的分离能力与开发纤维的优异灵敏度相结合,使我们能够在 ng/mL 范围内同时测定农药混合物。LOD 范围为 0.02-0.64 ng/mL。该方法成功地应用于选择性和灵敏地测定井水样品中目标农药,回收率值可接受(92-110%)。与商业纤维相比,聚噻吩纤维给出了令人满意的结果。选择了不同极性的常用农药作为代表性化合物,以搜索纤维对从葡萄园采集的井水分析的适用性。