Bagheri Habib, Soofi Gohar, Javanmardi Hasan, Karimi Majid
Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran.
Polymerization Engineering Department, Iran Polymer and Petrochemical Institute (IPPI), P.O. Box 14965/115, Tehran, Iran.
Mikrochim Acta. 2018 Aug 17;185(9):418. doi: 10.1007/s00604-018-2950-z.
Polyhedral oligomeric silsesquioxanes are 3D nanoscaled materials with large potential in solid phase microextraction (SPME). Here, as a case study, an octaglycidyldimethylsilyl modified polyhedral oligomeric silsesquioxane network is described. It was deposited on a stainless steel wire via a sol-gel method and used as a fiber coating for SPME of aromatic compounds. The uniform pore structure, high surface area, and hydrophobicity of the network make it susceptible toward isolation of non-polar and semi-polar chemical compounds. The performance of the fiber coating was tested with three classes of environmental pollutants, viz. chlorobenzenes (CBs), benzenes (benzene, toluene, ethylbenzene, xylene; known as BTEX), and polycyclic aromatic hydrocarbons. The effects of various types of sol-gel precursors on the fabrication and performance of fiber coatings were investigated. The extraction capability of the fiber coating was compared with the polydimethyl siloxane/divinylbenzene based commercial fiber. Parameters affecting headspace analysis and gas chromatographic quantitation were optimized. The method was applied to the quantification of PAHs, as model analytes, in tea, coffee and some environmental waters. Linear responses typically cover the 1-200 ng·L concentration range, limits of detection are between 0.1 and 0.3 ng·L, intra-day relative standard deviation are <10%, and inter-day RSDs are <12%. The fiber has a long lifespan and can be used >200 times. Graphical abstract Schematic presentation of a headspace solid phase microextraction process which is implemented to the analysis of PAHs in tea and coffee samples. The SEM image of the SPME fiber coating, the 3D nanoscale polyhedral oligomeric silsesquioxane (POSS) network, and the POSS-epoxy molecular structure are shown.
多面体低聚倍半硅氧烷是一类具有三维纳米尺度的材料，在固相微萃取（SPME）领域具有巨大潜力。在此，作为一个案例研究，描述了一种八缩水甘油基二甲基硅烷基改性的多面体低聚倍半硅氧烷网络。它通过溶胶 - 凝胶法沉积在不锈钢丝上，并用作芳香族化合物SPME的纤维涂层。该网络均匀的孔结构、高比表面积和疏水性使其易于分离非极性和半极性化合物。用三类环境污染物对该纤维涂层的性能进行了测试，即氯苯（CBs）、苯类（苯、甲苯、乙苯、二甲苯；即BTEX）和多环芳烃。研究了各种类型的溶胶 - 凝胶前驱体对纤维涂层制备和性能的影响。将该纤维涂层的萃取能力与基于聚二甲基硅氧烷/二乙烯基苯的商用纤维进行了比较。对影响顶空分析和气相色谱定量的参数进行了优化。该方法应用于茶叶、咖啡和一些环境水样中作为模型分析物的多环芳烃的定量分析。线性响应通常覆盖1 - 200 ng·L的浓度范围，检测限在0.1至0.3 ng·L之间，日内相对标准偏差<10%，日间相对标准偏差<12%。该纤维具有较长的使用寿命，可使用>200次。图形摘要：用于茶叶和咖啡样品中多环芳烃分析的顶空固相微萃取过程的示意图。展示了SPME纤维涂层的扫描电子显微镜图像、三维纳米尺度的多面体低聚倍半硅氧烷（POSS）网络以及POSS - 环氧树脂分子结构。
