Kermani Mansoure, Jafari Mohammad T, Saraji Mohammad
Department of Chemistry, Isfahan University of Technology, Isfahan 84156-83111, Iran.
Anal Methods. 2021 Jun 21;13(23):2631-2644. doi: 10.1039/d1ay00595b. Epub 2021 May 25.
A mesh screen was electrochemically coated with polypyrrole and used as a sorptive extractor device, for the first time. This configuration acts in such a way that it is self-rotating in the presence of a magnetic force and can be used for extraction and concentration of analytes. Actually, applying a mesh screen instead of a bar or plate in sorptive extraction provided a more effective contact area between the sorptive materials and sample solution, resulting in higher sorption efficiency. The device performance was assessed by using chlorpyrifos pesticide as a model analyte. A thermal desorption unit was coupled to an ion mobility spectrometer and applied for evaporating the extracted analyte. Different parameters affecting the extraction efficiency during the electro-polymerization and the extraction process, including the time of electrodeposition, the concentration of pyrrole, oxalic acid and salt, temperature and time of extraction, and the stirring rate of the extractor device were investigated and optimized, simultaneously. The detection and quantification limits of the method were calculated to be 0.035 and 0.1 μg L, respectively. The linear dynamic range obtained was from 0.1 to 20 μg L, with a determination coefficient of 0.9984. The intra-day and inter-day-relative standard deviations (RSD, n = 3) were lower than 3% and 8%, respectively. Under the optimal conditions, the absolute recovery and the enrichment factor were found to be 97% and 5820, respectively. Finally, the relative recoveries of the proposed method were calculated to be in the range of 86-111% for spiked water, wastewater, and apple samples. The results obtained from the method were validated by EPA method 622.
首次将一个筛网进行聚吡咯电化学涂层处理,并用作吸附萃取装置。这种结构在磁力作用下会自行旋转,可用于分析物的萃取和浓缩。实际上,在吸附萃取中使用筛网而非棒材或板材,能使吸附材料与样品溶液之间的接触面积更有效,从而提高吸附效率。以毒死蜱农药作为模型分析物评估了该装置的性能。将热解吸单元与离子迁移谱仪联用,用于蒸发萃取的分析物。同时研究并优化了在电聚合和萃取过程中影响萃取效率的不同参数,包括电沉积时间、吡咯、草酸和盐的浓度、萃取温度和时间以及萃取装置的搅拌速率。该方法的检测限和定量限分别计算为0.035和0.1 μg/L。获得的线性动态范围为0.1至20 μg/L,测定系数为0.9984。日内和日间相对标准偏差(RSD,n = 3)分别低于3%和8%。在最佳条件下,绝对回收率和富集因子分别为97%和5820。最后,该方法对加标水、废水和苹果样品的相对回收率计算结果在86 - 111%范围内。该方法得到的结果通过EPA方法622进行了验证。