School of Chemistry, Sun Yat-sen University, Guangzhou, 510275, China.
School of Chemistry, Sun Yat-sen University, Guangzhou, 510275, China.
J Chromatogr A. 2019 Jun 7;1594:45-53. doi: 10.1016/j.chroma.2019.02.038. Epub 2019 Feb 16.
Conjugated microporous polymers (CMPs) with permanent microporosity and extended p-conjugated skeletons have recently shown the fascinating application in separation and enrichment. In this report, porphyrin CMP that possessed microporous structure and nitrogen-rich pyrrole building blocks was successfully synthesized by microwave-assisted method. Then, a novel coating based on porphyrin CMP was fabricated on silica fiber for efficient enrichment volatile organic acids (VOAs). The simulation showed the coating exhibited strong interaction with volatile organic acids based on charge transfer interaction, hydrogen bond and size effect. Hence, we proposed a method for determination of volatile organic acids in tobaccos by headspace solid-phase microextraction (HS-SPME) with porphyrin CMP coating by gas chromatography-mass spectrometry. The results showed that the coating provided high enrichment factors for VOAs ranging from 66,657 to 133,970 and low limits of detection from 4.6 to 22 ng/L. A good linearity was observed for propionic acid and crotonic acid ranging from 0.050 to 8.0 μg/L, 2-methylheptanoic acid ranging from 0.063 to 1.5 μg/L, others ranging from 0.025 to 3.0 μg/L with the determination coefficient (R) between 0.9900 and 0.9980. The strategy for determination of volatile compounds in complex solid samples was successfully applied to the analysis of volatile organic acids in tobacco leaves. The results showed that the method was accurate and reliable.
具有永久微孔和扩展 p 共轭骨架的共轭微孔聚合物（CMPs）最近在分离和富集方面显示出了迷人的应用。在本报告中，通过微波辅助方法成功合成了具有微孔结构和富氮吡咯砌块的卟啉 CMP。然后，在硅胶纤维上制备了基于卟啉 CMP 的新型涂层，用于有效富集挥发性有机酸（VOAs）。模拟表明，该涂层基于电荷转移相互作用、氢键和尺寸效应与挥发性有机酸表现出强烈的相互作用。因此，我们提出了一种通过顶空固相微萃取（HS-SPME）与卟啉 CMP 涂层结合气相色谱-质谱法测定烟草中挥发性有机酸的方法。结果表明，该涂层对挥发性有机酸的富集因子高达 66,657 至 133,970，检测限低至 4.6 至 22 ng/L。丙酸和巴豆酸的线性良好，范围为 0.050 至 8.0 μg/L，2-甲基庚酸的线性良好，范围为 0.063 至 1.5 μg/L，其他的线性良好，范围为 0.025 至 3.0 μg/L，相关系数（R）在 0.9900 到 0.9980 之间。该用于复杂固体样品中挥发性化合物测定的策略成功应用于烟叶中挥发性有机酸的分析。结果表明，该方法准确可靠。
