College of Chemistry and Chemical Engineering, Jishou University, Hunan, Jishou 416000, China.
College of Chemistry and Chemical Engineering, Jishou University, Hunan, Jishou 416000, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2024 Feb 1;1233:123986. doi: 10.1016/j.jchromb.2023.123986. Epub 2023 Dec 29.
A [BMIM]PF ion liquid (IL)-assisted synthesis of a rutin imprinted monolith (RIM) was carried out in an in-situ polymerization method. Bi-functional monomers and a ternary porogen containing IL was used for the RIM preparation and a L(3) orthogonal factor design performed. Scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FT-IR) and N adsorption method was for structural characterization of the RIMs. The monolith was directly used as stationary phase in liquid chromatography to test the retention selectivity, adsorption capacity and extraction application. The optimized porogen consists of 900 μL DMF, 144 μL ACN and 216 μL IL. The monolith RIM-13 obtained under the optimized conditions possessed improved adsorption performance, with a dynamic adsorption capacity of 6.695 mg/g, an imprinting efficiency of 4.841 and a selectivity α value of 4.821. Additionally, this monolith had also higher specific surface area, pore volume and permeability than that obtained without IL and the homogeneity of the imprint sites could be improved by using IL. When the RIM-13 was applied to the separation and purification of rutin from tartary buckwheat, a rutin product with a purity higher than 92 % can be obtained by one cycle. This molecular imprint solid-phase extraction (MI-SPE) is of potency to be applied to preparative-scale separation of other natural products.
采用原位聚合法,以[BMIM]PF6 离子液体(IL)辅助合成芦丁印迹整体柱(RIM)。采用双功能单体和含有 IL 的三元致孔剂制备 RIM,并进行 L(3)正交因子设计。扫描电子显微镜(SEM)、傅里叶变换红外光谱(FT-IR)和 N 吸附法用于 RIM 的结构表征。整体柱直接用作液相色谱中的固定相,以测试保留选择性、吸附容量和萃取应用。优化的致孔剂由 900 μL DMF、144 μL ACN 和 216 μL IL 组成。在优化条件下得到的整体柱 RIM-13 具有改善的吸附性能,动态吸附容量为 6.695mg/g,印迹效率为 4.841,选择性α值为 4.821。此外,与不使用 IL 相比,该整体柱具有更高的比表面积、孔体积和渗透性,并且使用 IL 可以改善印迹位点的均一性。当 RIM-13 应用于从苦荞中分离和纯化芦丁时,通过一个循环可以得到纯度高于 92%的芦丁产物。这种分子印迹固相萃取(MI-SPE)具有应用于其他天然产物制备规模分离的潜力。