Magnetic molecularly-imprinted microspheres with a core-shell structure for the extraction of catalpol from both Rehmannia glutinosa Libosch and biological samples

梓醇 化学 地黄 分子印迹聚合物 色谱法 吸附 高效液相色谱法 磁性纳米粒子 傅里叶变换红外光谱 萃取(化学) 固相萃取 分析化学(期刊) 化学工程 纳米技术 选择性 材料科学 纳米颗粒 有机化学 糖苷 医学 替代医学 中医药 病理 工程类 催化作用
作者
Bing Qin,Xiaoyan Yu,Mingyuan Gao,Yanyan Zhang,Chunling Wang,Hongle Wan,Li Li,Mina Zhang,Mina Zhang,Weidong Zhang
出处
期刊:Journal of Chromatography A [Elsevier]
卷期号:: 464183-464183
标识
DOI:10.1016/j.chroma.2023.464183
摘要

We report on the successful development of a magnetic molecularly imprinted polymer (MMIP) for the separation and detection of catalpol in Rehmannia glutinosa extract and biological samples. Catalpol was used as the template molecule for the MMIPs, which were synthesized using the reverse prediction approach and differential UV-visible spectra to optimize the synthesis conditions. The resulting MMIPs were characterized using techniques including scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, and vibrating sample magnetometry, which confirmed their excellent nuclear shell construction and simple rapid magnetic separation. Static and dynamic adsorption experiments were performed to assess the sensitivity, repeatability, and adsorption capacity of the MMIPs. Adsorption capacity was found to be high (59.09 µg/mg). The MMIPs also exhibited strong identification specificity for catalpol analogs (IF = 2.41). Magnetic solid phase extraction (MSPE) was optimized to establish an MSPE-HPLC approach based on the MMIPs. Under ideal conditions, the new method showed excellent determination coefficient (R2 > 0.99) in the ranges of 0.1–1.0 mg/mL and 0.03–0.18 mg/mL for R. glutinosa extract and biological material, respectively, with limits of detection of 5.4 ng/mL and 1.7 ng/mL. The novelty of this research lies in the preparation of magnetic surface MMIPs using a magnetic carrier. These MMIPs exhibit excellent magnetic properties and possess specific adsorption capability for catalpol, enabling rapid separation. They offer advantages such as low cost, high specificity, chemical stability, physical robustness, and recyclability (97.09%–106.53%, 91.32%–100.99%). The application of these polymers in the pretreatment method for determining the catalpol content in R. glutinosa extract and biological samples enhances the extraction efficiency and detection accuracy for catalpol. It eliminates interference and influences from other components in catalpol determination while exhibiting high sensitivity, good enrichment effects, excellent reusability, and a high recovery rate.
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