Department of Chemistry, Isfahan University of Technology, Isfahan 84156-83111, Iran.
J Chromatogr A. 2013 Mar 1;1279:20-6. doi: 10.1016/j.chroma.2013.01.017. Epub 2013 Jan 10.
A novel solid-phase microextraction (SPME) fiber coated with polypyrrole/sol-gel composite was prepared through electrochemical deposition. The composite polymer coating was prepared using a three-electrode electrochemical system and directly deposited on a stainless steel wire by applying a constant potential (1.2V for 1000 s). The coating has porous surface structure, stable performance in high temperature, and good coating preparation reproducibility. The SPME composite coating was evaluated by analyzing some organophosphorus pesticides (OPPs) in water and vegetable samples followed by gas chromatography and nitrogen phosphorus detection. Different SPME parameters influencing the extraction efficiency such as coating thickness, salt concentration, stirring rate, extraction time and temperature, desorption time and desorption temperature were investigated. Under the optimized conditions, the coating showed better extraction efficiency than polypyrrole and commercial SPME fibers. The detection limits were 1.5-10 ng L(-1). Relative standard deviations for intra- and inter-day precision for a single fiber were in the range of 1.1-2.9% and 2.2-4.2%, respectively. Fiber to fiber reproducibility was in the range of 6.0-10.1% (n=3). The calibration curves were linear in the concentration range from 5 to 2000 ng L(-1) (r(2)>0.9953). Finally, the developed method was applied for the analysis of cucumber, lettuce, tap and well water samples and the relative recovery was found to be in the range of 80-109%, at the optimum conditions.
一种新型的聚吡咯/溶胶-凝胶复合固相微萃取(SPME)纤维是通过电化学沉积制备的。复合聚合物涂层是在三电极电化学系统中制备的,通过施加恒电位(1.2V 持续 1000s)直接沉积在不锈钢丝上。该涂层具有多孔表面结构、高温稳定性和良好的涂层制备重现性。通过气相色谱和氮磷检测分析水样和蔬菜样品中的一些有机磷农药(OPPs),对 SPME 复合涂层进行了评价。研究了不同的 SPME 参数对萃取效率的影响,如涂层厚度、盐浓度、搅拌速度、萃取时间和温度、解吸时间和解吸温度。在优化条件下,该涂层的萃取效率优于聚吡咯和商用 SPME 纤维。检测限为 1.5-10ngL(-1)。单个纤维的日内和日间精密度的相对标准偏差分别在 1.1-2.9%和 2.2-4.2%之间。纤维间的重现性在 6.0-10.1%(n=3)之间。校准曲线在 5-2000ngL(-1)浓度范围内呈线性(r(2)>0.9953)。最后,该方法应用于黄瓜、生菜、自来水和井水样品的分析,在最佳条件下,相对回收率在 80-109%之间。