Rahimi M, Noroozian E
Department of Chemistry, Shahid Bahonar University of Kerman, Kerman, Iran; Young Researchers Society, Shahid Bahonar University of Kerman, P.O. Box 76169-133, Kerman, Iran.
Department of Chemistry, Shahid Bahonar University of Kerman, Kerman, Iran.
Anal Chim Acta. 2014 Jul 11;836:45-52. doi: 10.1016/j.aca.2014.05.040. Epub 2014 May 28.
A conducting copolymer of pyrrole and phenol was electrochemically synthesized on steel frits as a sorbent. The applicability of the frit was assessed for the solid-phase extraction of trace amounts of polycyclic aromatic hydrocarbons (PAHs) in aqueous samples followed by HPLC-UV. The coating produced was very adherent and the scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and FTIR spectrum for the coated frit were studied. The effects of various parameters on the efficiency of the solid-phase extraction process, such as the sample loading rate, elution solvent type, salt effect, volume and flow rate of sample and elution solvent were investigated. Under the optimal conditions, the calibration curves were obtained in the range of 0.1-500ngmL(-1) (r(2)>0.98) and the LODs (S/N=3) were obtained in the range of 0.01-0.08ngmL(-1). Relative standard deviations (RSDs) for intra- and inter-day precision were 2.7-10.2% and 3.6-11.4%, respectively. The recoveries (8 and 40ngmL(-1)) ranged from 79% to 115%. The simplicity of experimental procedure, short sample analysis, high extraction efficiency, and the use of low-cost adsorbent show the potential of this method for routine analysis of PAHs in real samples.
在钢筛上通过电化学合成制备了吡咯和苯酚的导电共聚物作为吸附剂。评估了该筛在高效液相色谱-紫外检测法（HPLC-UV）之前对水样中痕量多环芳烃（PAHs）进行固相萃取的适用性。研究了所制备涂层的附着力，并对涂覆筛进行了扫描电子显微镜（SEM）、能量色散X射线光谱（EDX）和傅里叶变换红外光谱（FTIR）分析。考察了各种参数对固相萃取效率的影响，如样品加载速率、洗脱溶剂类型、盐效应、样品和洗脱溶剂的体积及流速。在最佳条件下，校准曲线在0.1-500ngmL(-1)范围内获得（r(2)>0.98），检测限（S/N=3）在0.01-0.08ngmL(-1)范围内。日内和日间精密度的相对标准偏差（RSDs）分别为2.7-10.2%和3.6-11.4%。回收率（8和40ngmL(-1)）在79%至115%之间。实验步骤简单、样品分析时间短、萃取效率高以及使用低成本吸附剂表明了该方法在实际样品中PAHs常规分析方面的潜力。
