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Ultra-trace determination of polycyclic aromatic hydrocarbons using solid-phase extraction coupled with HPLC based on graphene-functionalized silica gel composites

机译:基于石墨烯官能化硅胶复合物的固相萃取-HPLC结合超痕量测定多环芳烃

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摘要

A graphene (Gr) functionalized silica gel (Gr-SiO2) sorbent was prepared and used as a new sorbent for solid-phase extraction (SPE) of polycyclic aromatic hydrocarbons (PAHs) including naphthalene, acenaphthylene, fluorene, phenanthrene, fluoranthene, and pyrene. The analytes were separated and detected by high-performance liquid chromatography (HPLC) with a UV detector. Factors affecting the extraction efficiency including the eluent type and its volume, adsorbent amount, sample volume, sample pH and flow rate were optimized. Under the optimized conditions, the present method showed a wide linear range (0.01-600 μg L~(-1)), acceptable repeatability of the extraction (RSDs of 1.7-8.2%, n = 3) and satisfactory detection limits (0.0029-0.052 μg L~(-1)). The recovery studies using this new sorbent were performed by three consecutive extraction steps of water and milk samples at three spiked levels. The average recoveries of the analytes in environmental water and milk samples were 89.0-115.4%, which demonstrated the applicability of the developed method.
机译:制备了石墨烯(Gr)官能化硅胶(Gr-SiO2)吸附剂并将其用作固相萃取(SPE)多环芳烃(PAH)的新型吸附剂,包括萘,,芴,菲,荧蒽和new 。分离出分析物,并通过带有UV检测器的高效液相色谱(HPLC)进行检测。优化了影响萃取效率的因素,包括洗脱液类型及其体积,吸附剂量,样品体积,样品pH值和流速。在优化的条件下,本方法显示出宽线性范围(0.01-600μgL〜(-1)),可接受的萃取重复性(RSD为1.7-8.2%,n = 3)和令人满意的检测限(0.0029- 0.052μgL〜(-1))。使用这种新吸附剂的回收率研究是通过三个加标水平的水和牛奶样品的三个连续提取步骤进行的。环境水和牛奶样品中分析物的平均回收率为89.0-115.4%,证明了该方法的适用性。

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