Fabrication of cross-linked hydrazone covalent organic frameworks by click chemistry and application to solid phase microextraction.
Fabrication of cross-linked hydrazone covalent organic frameworks by click chemistry and application to solid phase microextraction.
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DOI：
10.1016/j.talanta.2016.08.041
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发表时间：
2016-12
期刊：
影响因子：
6.1
通讯作者：
Mingxue Wu;Gang Chen;Jiutong Ma;Ping Liu;Q. Jia
中科院分区：
文献类型：
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作者：
Mingxue Wu;Gang Chen;Jiutong Ma;Ping Liu;Q. Jia
共价有机骨架材料是一类新兴的多孔有机骨架材料，具有广泛的应用前景。本文首次提出了一种基于巯基-烯点击化学的交联腙COFs固相微萃取（SPME）。所制备的网络具有较强的共价键和层间性，保证了新型SPME纤维的吸附能力和耐久性。交联COFs中含有大量的苯环和-C=N基团，存在π-π共轭结构。一系列表征结果表明，交联COFs具有大的比表面积、高的孔隙率、高的稳定性和良好的疏水性。将该光纤应用于农药残留的固相微萃取-气相色谱-电子捕获检测器（GC-ECD）联用。在最佳实验条件下，强化因子在2190-10,998之间，表明交联COFs具有良好的富集能力。低检测限为0.0003-0.0023 ng kg− 1，相对标准偏差（RSD）分别为3.4-7.6%（批内）和5.7-11.6%（批间）。将SPME-GC法应用于黄瓜样品中农药残留的分析，回收率在78.2%-107.0%之间。
Covalent organic frameworks (COFs) are an emerging class of porous organic frameworks with diverse promising applications. Herein, we presented the first example of cross-linked hydrazone COFs (cross-linked COFs) coatingviathiol-ene click chemistry for solid phase microextraction (SPME). Strong covalent bonds and interlayer of the prepared networks ensured the adsorption capacity and durability of the novel SPME fiber. π-π conjugated structure existed because of abundant phenyl rings and –C=N groups in the cross-lined COFs. A series of characterizations indicated that the cross-linked COFs possessed large surface areas, high porosities and stabilities as well as hydrophobicities. The fiber was applied to SPME of pesticide residues coupled with gas chromatography with an electron capture detector (GC-ECD). Under the optimum experimental conditions, enhancement factors in the range of 2190–10,998 were obtained, illustrating that the cross-linked COFs possessed remarkable preconcentration ability. The low detection limits of 0.0003–0.0023 ng kg−1were achieved with relative standard deviations (RSDs) in the range of 3.4–7.6% (intra-batch) and 5.7–11.6% (inter-batch), respectively. Recovery values in the range of 78.2–107.0% were obtained when the SPME-GC method was applied to the analysis of pesticides in cucumber samples.