Departamento de Química Inorgánica y Analítica, Facultad de Ciencias Químicas y Farmacéuticas, Universidad de Chile, Sergio Livingstone 1007, Santiago, Casilla 233, Chile.
Talanta. 2012 Oct 15;100:439-46. doi: 10.1016/j.talanta.2012.08.015. Epub 2012 Aug 18.
The potential of microwave-assisted liquid-liquid and solid phase extraction coupled with fluorescence spectroscopy and employing one- to three-way spectral data was assessed in terms of their capacity for the rapid detection of heavy polycyclic aromatic hydrocarbons (PAHs) in olive and sunflower oils. Tocopherols and pigments groups (chlorophyll and pheophytin) present in oil matrices were the main interference compounds in the detection of PAHs using fluorescence spectroscopy. Partial spectral overlap and inner-filter effects were observed in the emission range of the analytes. The effectiveness of removing these interferences using solid phase extraction (silica, C18 and graphitized carbon black) was examined. Solid phase extraction with silica was the most effective method for the removal of pigments and tocopherol and allowed for the detection of PAHs in edible oils using fluorescence spectroscopy. The limit of detection was observed to depend on the use of one-, two- or three-way fluorescence spectral data in the range of 0.8 to 7.0 μg kg(-1). The individual recoveries of PAHs following the microwave-assisted L-L extraction and SPE with silica were assessed using HPLC-FD with satisfactory results.
采用微波辅助液-液和固相萃取与荧光光谱法相结合,并利用单至三谱数据,评估了其快速检测橄榄油和葵花籽油中多环芳烃(PAHs)的潜力。油基质中的生育酚和色素组(叶绿素和脱镁叶绿素)是荧光光谱法检测 PAHs 的主要干扰化合物。在分析物的发射范围内观察到部分光谱重叠和内滤效应。考察了使用固相萃取(硅胶、C18 和石墨化炭黑)去除这些干扰的效果。硅胶固相萃取是去除色素和生育酚最有效的方法,允许使用荧光光谱法检测食用油中的 PAHs。检测限观察到取决于在 0.8 至 7.0μgkg(-1) 范围内使用单、双或三谱荧光数据。使用 HPLC-FD 评估了微波辅助 L-L 萃取和硅胶 SPE 后 PAHs 的单独回收率,结果令人满意。