Li Xiang, Chen Jianmin, Du Lichun
Department of Environmental Science & Engineering, Fudan University, Shanghai 200433, China.
J Chromatogr A. 2007 Jan 26;1140(1-2):21-8. doi: 10.1016/j.chroma.2006.11.044. Epub 2006 Nov 30.
A simple solid-phase microextraction (SPME) device, coupled with gas chromatography-electron capture detection (GC-ECD) was developed to detect trace levels of chloro- and nitrobenzene compounds in environmental water samples. Polyaniline (PANI) was chosen as the extraction material for the SPME device, and was electrochemically deposited on a stainless steel wire to achieve high mechanical stability. Due to the peculiar pi-pi conjugated structure, PANI coating shows a stable performance in high temperature (to 350 degrees C) and solvents (organic and inorganic). The porous structure of PANI film characterized by scanning electron microscopy (SEM) revealed high extraction efficiency. The possible extraction mechanism was explained by the study carried out using electrochemical impedance spectroscopy (EIS). Eight chloro- and nitrobenzene compounds were selected to evaluate the SPME-GC procedures. The key parameters such as extraction and desorption temperature and time, and the ionic strength were investigated and optimized. The method was applied to the detection of environmental water samples collected from Taihu Lake, representing nowadays contamination level under industrial impact. The whole PANI-SPME-GC method offers high accuracy and precision, high sensitivity and low detection limits. Thus, the method developed could be used as a new way to monitor the trace levels of chloro- and nitrobenzene compounds in real water bodies.
开发了一种简单的固相微萃取(SPME)装置,与气相色谱 - 电子捕获检测(GC - ECD)联用,用于检测环境水样中痕量的氯苯和硝基苯化合物。选择聚苯胺(PANI)作为SPME装置的萃取材料,并将其电化学沉积在不锈钢丝上以实现高机械稳定性。由于其独特的π-π共轭结构,聚苯胺涂层在高温(至350℃)和溶剂(有机和无机)中表现出稳定的性能。通过扫描电子显微镜(SEM)表征的聚苯胺膜的多孔结构显示出高萃取效率。使用电化学阻抗谱(EIS)进行的研究解释了可能的萃取机制。选择了八种氯苯和硝基苯化合物来评估SPME - GC程序。研究并优化了萃取和解吸温度和时间以及离子强度等关键参数。该方法应用于检测从太湖采集的环境水样,代表了当今工业影响下的污染水平。整个聚苯胺 - SPME - GC方法具有高准确度和精密度、高灵敏度和低检测限。因此,所开发的方法可作为监测实际水体中痕量氯苯和硝基苯化合物的新方法。