Ege University, Faculty of Science, Department of Chemistry, Bornova, Izmir, Turkey.
Ege University, Faculty of Science, Department of Chemistry, Bornova, Izmir, Turkey.
Anal Chim Acta. 2015 Feb 15;859:37-45. doi: 10.1016/j.aca.2014.12.043. Epub 2014 Dec 26.
This report comprises the novel usage of polythiophene - ionic liquid modified clay surfaces for solid phase microextraction (SPME) fiber production to improve the analysis of pesticides in fruit juice samples. Montmorillonite (Mmt) clay intercalated with ionic liquids (IL) was co-deposited with polythiophene (PTh) polymer coated electrochemically on an SPME fiber. The surface of the fibers were characterized by using scanning electron microscopy (SEM). Operational parameters effecting the extraction efficiency namely; the sample volume and pH, adsorption temperature and time, desorption temperature and time, stirring rate and salt amount were optimized. In order to reveal the major effects, these eight factors were selected and Plackett-Burman Design was constructed. The significant parameters detected; adsorption and temperature along with the stirring rate, were further investigated by Box-Behnken design. Under optimized conditions, calibration graphs were plotted and detection limits were calculated in the range of 0.002-0.667ng mL(-1). Relative standard deviations were no higher than 18%. Overall results have indicated that this novel PTh-IL-Mmt SPME surface developed by the aid of electrochemical deposition could offer a selective and sensitive head space analysis for the selected pesticide residues.
本报告包括聚噻吩-离子液体修饰的粘土表面在固相微萃取（SPME）纤维生产中的新用途，以改善果汁样品中农药的分析。蒙脱土（Mmt）粘土与离子液体（IL）插层共沉积，聚噻吩（PTh）聚合物在 SPME 纤维上电化学涂覆。使用扫描电子显微镜（SEM）对纤维的表面进行了表征。优化了影响萃取效率的操作参数，即样品体积和 pH 值、吸附温度和时间、解吸温度和时间、搅拌速度和盐量。为了揭示主要影响，选择了这 8 个因素并构建了 Plackett-Burman 设计。检测到的显著参数；吸附和温度以及搅拌速度，通过 Box-Behnken 设计进一步进行了研究。在优化条件下，绘制了校准曲线，并在 0.002-0.667ng mL（-1）范围内计算了检测限。相对标准偏差不高于 18%。总体结果表明，这种新型的 PTh-IL-Mmt SPME 表面通过电化学沉积的辅助开发，可以为所选农药残留物提供选择性和灵敏的顶空分析。
