Abboud Ayad Sami, Sanagi Mohd Marsin, Ibrahim Wan Aini Wan, Keyon Aemi S Abdul, Aboul-Enein Hassan Y
Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia.
Ministry of Construction, Housing and Public Municipalities, Baghdad 10003, Iraq.
J Chromatogr Sci. 2018 Feb 1;56(2):177-186. doi: 10.1093/chromsci/bmx095.
In this study, caged calcium alginate-caged multiwalled carbon nanotubes dispersive microsolid phase extraction was described for the first time for the extraction of polycyclic aromatic hydrocarbons (PAHs) from water samples prior to gas chromatographic analysis. Fluorene, phenanthrene and fluoranthene were selected as model compounds. The caged calcium alginate-caged multiwalled carbon nanotubes was characterized by Fourier transform infrared spectroscopy, scanning electron microscopy and thermal gravimetry analyses. The effective parameters namely desorption solvent, solvent volume, extraction time, desorption time, the mass of adsorbent and sample volume were optimized. Under the optimum extraction conditions, the developed method showed good linearity in the range of 0.5-50 ng mL-1 (R2 ≥ 0.996), low limits of detection and quantification (0.42-0.22 ng mL-1) (0.73-1.38 ng mL-1) respectively, good relative recoveries (71.2-104.2%) and reproducibility (RSD 1.8-12.4%, n = 3) for the studied PAHs in water sample. With high enrichment factor (1,000), short extraction time (<30 min), low amounts of adsorbent (100 mg) and low amounts of solvent (0.1 mol) have proven that the microsolid phase extraction method based on calcium alginate-caged multiwalled carbon nanotubes are environmentally friendly and convenient extraction method to use as an alternative adsorbent in the simultaneous preconcentration of PAHs from environmental water samples.
在本研究中，首次描述了笼形海藻酸钙包裹多壁碳纳米管分散微固相萃取法，用于在气相色谱分析之前从水样中萃取多环芳烃（PAHs）。选择芴、菲和荧蒽作为模型化合物。通过傅里叶变换红外光谱、扫描电子显微镜和热重分析对笼形海藻酸钙包裹多壁碳纳米管进行了表征。对解吸溶剂、溶剂体积、萃取时间、解吸时间、吸附剂质量和样品体积等有效参数进行了优化。在最佳萃取条件下，所建立的方法在0.5 - 50 ng mL-1范围内具有良好的线性（R2≥0.996），检测限和定量限分别较低（0.42 - 0.22 ng mL-1）（0.73 - 1.38 ng mL-1），对于水样中所研究的PAHs具有良好的相对回收率（71.2 - 104.2%）和重现性（RSD 1.8 - 12.4%，n = 3）。该方法具有高富集因子（1000）、短萃取时间（<30分钟）、低吸附剂用量（100 mg）和低溶剂量（0.1 mol），证明基于海藻酸钙包裹多壁碳纳米管的微固相萃取方法是一种环保且方便的萃取方法，可作为从环境水样中同时预富集PAHs的替代吸附剂。
