Department of Chemistry, College of Science, Princess Nourah bint Abdulrahman University, Riyadh, Saudi Arabia; Deanship of Scientific Research, Princess Nourah bint Abdulrahman University, Riyadh, Saudi Arabia.
Department of Chemistry, College of Science, King Saud University, Riyadh, Saudi Arabia.
J Chromatogr A. 2018 Feb 2;1535:17-26. doi: 10.1016/j.chroma.2018.01.011. Epub 2018 Jan 4.
A composite of multi-walled carbon nanotubes incorporated into a benzyl methacrylate-co-ethylene dimethacrylate porous monolith was prepared, characterized and used as solid phase adsorbent and as stationary phase for simultaneous extraction and separation of ten polycyclic aromatic hydrocarbons, followed by nano-liquid chromatography analysis. The extraction and chromatographic parameters were optimized with regard to the extraction efficiency and the quality of chromatographic analytes separation. Under the optimized conditions, all PAHs were separated in 13 min with suitable resolution values (Rs = 1.74-3.98). Addition of a small amount of carbon nanotubes (0.1% with respect to monomers) to the polymerization mixture increased the efficiency for the separation column to over 41,700 plates m for chrysene at flow rate of 0.5 μL min. The method showed a wide linear range (1-500 μg L with R more than 0.9938), acceptable extraction repeatability (RSDs < 6.4%, n = 3) and reproducibility (RSDs < 12.6%, five parallel-made solid phase extraction cartridges) and satisfactory detection limits (0.02-0.22 μg L). Finally, the proposed method was successfully applied to the detection of polycyclic aromatic hydrocarbons in environmental water samples. After a simple extraction procedure with preconcentration factor equal to 100, the average recovery values in ultra-pure, tap and sea water samples were found to be in the range 81.3-95.4% with %RSD less than 6.4. Again, the presence of carbon nanotubes (0.3% relatively to monomers) in native polymer enhanced the extraction performance for the solid phase adsorbent up to 78.4%. The application of the monoliths modified with CNTs in extraction and nano-scale liquid chromatography for analysis of environmental samples offered several advantages; it demonstrated an acceptable precision, low detection limits, good reproducibility, satisfying recoveries and wide dynamic linear ranges.
将多壁碳纳米管复合材料掺入苄基甲基丙烯酸酯-乙二醇二甲基丙烯酸酯多孔单体中，制备、表征并用作固相吸附剂和同时萃取和分离十种多环芳烃的固定相，然后进行纳流液相色谱分析。针对萃取效率和色谱分析物分离的质量，对萃取和色谱参数进行了优化。在优化条件下，所有多环芳烃在 13 分钟内以合适的分辨率值（Rs=1.74-3.98）分离。在聚合混合物中添加少量的碳纳米管（相对于单体的 0.1%）可将分离柱的效率提高到超过 41700 板/米，在流速为 0.5μL/min 时对荧蒽的分离效率。该方法具有较宽的线性范围（1-500μg/L，R 大于 0.9938）、可接受的萃取重复性（RSDs<6.4%，n=3）和重现性（RSDs<12.6%，五个平行制作的固相萃取小柱）和令人满意的检测限（0.02-0.22μg/L）。最后，该方法成功应用于环境水样中多环芳烃的检测。经过简单的萃取程序，浓缩因子等于 100，在超纯水、自来水和海水中的平均回收率在 81.3-95.4%之间，RSD 小于 6.4%。同样，在天然聚合物中添加 0.3%的碳纳米管（相对于单体）可将固相吸附剂的萃取性能提高到 78.4%。在提取和纳米级液相色谱分析中使用改性 CNT 的整体柱具有以下优点：它具有可接受的精度、低检测限、良好的重现性、令人满意的回收率和宽动态线性范围。
