Since the severe hazard to the ecosystem and widespread distribution through biological and man-made ways of polycyclic aromatic hydrocarbons (PAHs), it is very urgent to establish the ultrasensitive analytical method to quantitatively and directly monitor PAHs in real samples. However, because of the complicated environmental matrix and their trace concentration, the pre-concentration process is a necessary step to analyze of these compounds. In this study, solid phase microextraction (SPME) technique was proposed to separate and enrich fifteen trace PAHs from environmental samples. In this work, a honeycomb-like triazine-based conjugated microporous polymers (T-CMPs) were prepared by Yamamoto reaction and firstly used as SPME coating material for the ultrasensitive direct-immersion-SPME of PAHs prior to high performance liquid chromatography-fluorescence detector (HPLC-FLD). The synthesized T-CMPs was characterized using various spectroscopy and electron microscopy techniques. The unique porous network of T-CMPs might deliver abundant adsorption sites for PAHs. Orthogonal experimental design (OED) was used to investigate the influence of four experimental parameters on the enrichment ability. Under optimal situation, a wide linear range (which lasted from 0.003 to 1000 μg L) with the coefficients of determination (R) varying 0.9981 to 0.9993 was obtained. The limits of detection (LODs) for the analytes varied from 0.001 to 1.650 μg L, and the limits of quantification (LOQs) were between 0.003 and 4.960 μg L. The proposed method was effectively employed to the simultaneous and ultrasensitive detection of fifteen PAHs in industrial wastewaters. The relative recoveries for PAHs analysis varied from 74.6 % to 105 % with the relative standard deviations (RSD) of 0.1 %–7.5 % in real water samples. The prepared SPME coating material exhibited a simultaneous, high extraction and adsorption capacity for fifteen PAHs due to its honeycomb-like porous structure, ultra-large specific surface area, strong π-π stacking, and hydrophobic interactions. The present research developed a novel strategy for the construction of SPME fiber coating composites and demonstrated great application potential in the field of sample pretreatment and environmental analytical chemistry.

中文翻译：

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蜂窝状三嗪基共轭微孔聚合物采用固相微萃取技术同时超灵敏检测 15 种多环芳烃


由于多环芳烃(PAHs)对生态系统的严重危害以及通过生物和人为途径的广泛分布，迫切需要建立超灵敏的分析方法来定量、直接监测实际样品中的PAHs。然而，由于环境基质复杂且浓度微量，预浓缩过程是分析这些化合物的必要步骤。在本研究中，提出了固相微萃取（SPME）技术来从环境样品中分离和富集 15 种痕量多环芳烃。在这项工作中，通过山本反应制备了蜂窝状三嗪基共轭微孔聚合物（T-CMP），并首次用作多环芳烃超灵敏直接浸入式固相微萃取（SPME）涂层材料，用于高效液相色谱-荧光检测器(HPLC-FLD)。使用各种光谱学和电子显微镜技术对合成的 T-CMP 进行了表征。 T-CMP 独特的多孔网络可能为 PAH 提供丰富的吸附位点。采用正交实验设计（OED）研究四个实验参数对富集能力的影响。在最佳情况下，获得了较宽的线性范围（从0.003至1000μg·L），决定系数（R）在0.9981至0.9993之间变化。分析物的检测限 (LOD) 在 0.001 至 1.650 μg L 之间变化，定量限 (LOQ) 在 0.003 至 4.960 μg L 之间。所提出的方法可有效地用于同时和超灵敏地检测水中的 15 种 PAH。工业废水。 PAH 分析的相对回收率从 74.6% 到 105% 不等，相对标准偏差 (RSD) 为 0.1%–7。实际水样中为 5%。所制备的固相微萃取涂层材料由于其蜂窝状多孔结构、超大比表面积、强π-π堆积和疏水相互作用，对15种PAHs表现出同时、高萃取和吸附能力。本研究开发了一种构建固相微萃取纤维涂层复合材料的新策略，并在样品预处理和环境分析化学领域展示了巨大的应用潜力。