Amanzadeh Hatam, Yamini Yadollah, Moradi Morteza
Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175 Tehran, Iran.
Department of Semiconductors, Materials and Energy Research Center, Karaj, Iran.
Anal Chim Acta. 2015 Jul 16;884:52-60. doi: 10.1016/j.aca.2015.05.018. Epub 2015 May 14.
In this work, ZnO/PPy nanocomposite coating was fabricated on stainless steel and evaluated as a novel headspace solid phase microextraction (HS-SPME) fiber coating for extraction of ultra-trace amounts of environmental pollutants; namely, aliphatic hydrocarbons in water and soil samples. The ZnO/PPy nanocomposite were prepared by a two-step process including the electrochemical deposition of PPy on the surface of stainless steel in the first step, and the synthesis of ZnO nanorods by hydrothermal process in the pores of PPy matrix in the second step. Porous structure together with ZnO nanorods with the average diameter of 70 nm were observed on the surface by using scanning electron microscopy (SEM). The effective parameters on HS-SPME of hydrocarbons (i.e., extraction temperature, extraction time, desorption temperature, desorption time, salt concentration, and stirring rate) were investigated and optimized by one-variable-at-a-time method. Under optimized conditions (extraction temperature, 65±1°C; extraction time, 15 min; desorption temperature, 250°C; desorption time, 3 min; salt concentration, 10% w/v; and stirring rate, 1200 rpm), the limits of detection (LODs) were found in the range of 0.08-0.5 μg L(-1), whereas the repeatability and fiber-to-fiber reproducibility were in the range 5.4-7.6% and 8.6-10.4%, respectively. Also, the accuracies obtained for the spiked n-alkanes were in the range of 85-108%; indicating the absence of matrix effects in the proposed HS-SPME method. The results obtained in this work suggest that ZnO/PPy can be promising coating materials for future applications of SPME and related sample preparation techniques.
在本研究中,在不锈钢表面制备了ZnO/PPy纳米复合涂层,并将其作为一种新型的顶空固相微萃取(HS-SPME)纤维涂层,用于萃取超痕量环境污染物,即水和土壤样品中的脂肪烃。ZnO/PPy纳米复合材料通过两步法制备,第一步是在不锈钢表面电化学沉积PPy,第二步是在PPy基质的孔隙中通过水热法合成ZnO纳米棒。使用扫描电子显微镜(SEM)观察到表面存在多孔结构以及平均直径为70 nm的ZnO纳米棒。采用单变量法研究并优化了烃类HS-SPME的有效参数(即萃取温度、萃取时间、解吸温度、解吸时间、盐浓度和搅拌速率)。在优化条件下(萃取温度65±1°C;萃取时间15分钟;解吸温度250°C;解吸时间3分钟;盐浓度10% w/v;搅拌速率1200 rpm),检测限(LOD)在0.08 - 0.5 μg L(-1)范围内,而重复性和纤维间重现性分别在5.4 - 7.6%和8.6 - 10.4%范围内。此外,加标正构烷烃的回收率在85 - 108%范围内,表明所提出的HS-SPME方法不存在基质效应。本研究所得结果表明,ZnO/PPy有望成为未来SPME及相关样品制备技术应用的涂层材料。