Key Laboratory of Life-Organic Analysis of Shandong Province, Qufu Normal University, Qufu 273165, PR China.
Key Laboratory of Life-Organic Analysis of Shandong Province, Qufu Normal University, Qufu 273165, PR China.
J Chromatogr A. 2020 May 24;1619:460949. doi: 10.1016/j.chroma.2020.460949. Epub 2020 Feb 5.
In this work, a dispersive solid phase extraction (d-SPE) method for sulfonamides (SAs) has been developed using a stable and mesoporous metal organic framework (University in Oslo 67, UiO-67) as adsorbent, which was synthesized by coordination of Zr ions with 4, 4-biphenyl-dicarboxylicacid (HBPDC) through a facile one-pot method. Owing to the synergistic effects of π-π interaction, hydrogen bonding, hydrophobic interaction and size match between SAs and the adsorbent, the extraction performance of UiO-67 for SAs was obviously improved. The adsorption behavior, evaluated by the kinetic models, showed that the intraparticle diffusion was involved during the adsorption process. The proper match between the pore size of UiO-67 (3.49 nm) and the molecular sizes of SAs (1.1 nm × 0.65 nm) not only allowed SAs to diffuse intraparticle but also permitted them to adjust their configurations to form hydrogen bonding with the UiO-67. By combination with HPLC analysis, a simple, sensitive, accurate and precise method for detection of SAs has been established. The method proposed in this work showed good performances, including wide linearity (14.6-250 ng/g) with high correlation coefficients (R ≥ 0.9991), low limits of detection (LODs, 0.7-6.5 ng/g for all SAs), satisfactory precision (Intra-day RSDs ≤ 3.4%, inter-day RSDs ≤ 4.7%), and high accuracy (recovery: 83.4-103.8%). Furthermore, benefiting from the mesoporous structure and the Zr cluster center as well as the stability, UiO-67 shows great potential to be an excellent adsorbent of SPE for extraction of SAs from other complex matrices.
在这项工作中,开发了一种使用稳定的介孔金属有机骨架(奥斯陆大学 67,UiO-67)作为吸附剂的分散固相萃取(d-SPE)方法来萃取磺胺类药物(SAs),该吸附剂是通过Zr 离子与 4,4-联苯-二羧酸(HBPDC)的配位在一锅法中合成的。由于π-π 相互作用、氢键、疏水相互作用以及磺胺类药物与吸附剂之间的尺寸匹配的协同作用,UiO-67 对磺胺类药物的萃取性能得到了明显提高。通过动力学模型评价吸附行为表明,吸附过程中涉及内扩散。UiO-67 的孔径(3.49nm)与磺胺类药物的分子尺寸(1.1nm×0.65nm)之间的适当匹配不仅允许磺胺类药物在颗粒内扩散,而且允许它们调整构型以与 UiO-67 形成氢键。结合 HPLC 分析,建立了一种简单、灵敏、准确和精确的磺胺类药物检测方法。本工作提出的方法表现出良好的性能,包括宽线性范围(14.6-250ng/g,相关系数 R≥0.9991)、低检测限(LODs,所有磺胺类药物的检测限为 0.7-6.5ng/g)、令人满意的精密度(日内 RSDs≤3.4%,日间 RSDs≤4.7%)和高准确度(回收率:83.4-103.8%)。此外,得益于介孔结构和 Zr 簇中心以及稳定性,UiO-67 有望成为从其他复杂基质中萃取磺胺类药物的 SPE 的优秀吸附剂。