PMID- 37454456 OWN - NLM STAT- MEDLINE DCOM- 20230809 LR - 20230809 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1705 DP - 2023 Aug 30 TI - Magnetic molecularly-imprinted microspheres with a core-shell structure for the extraction of catalpol from both Rehmannia glutinosa Libosch and biological samples. PG - 464183 LID - S0021-9673(23)00409-0 [pii] LID - 10.1016/j.chroma.2023.464183 [doi] AB - 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 microg/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 (R(2) > 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. CI - Copyright (c) 2023. Published by Elsevier B.V. FAU - Qin, Bing AU - Qin B AD - School of Pharmaceutical Sciences, Jilin University, Changchun, China; School of Pharmaceutical Sciences, Jiamusi University, Jiamusi, China. FAU - Yu, Xiaoyan AU - Yu X AD - School of Pharmaceutical Sciences, Jilin University, Changchun, China. FAU - Gao, Mingyuan AU - Gao M AD - School of Pharmaceutical Sciences, Jilin University, Changchun, China. FAU - Zhang, Yanyan AU - Zhang Y AD - School of Pharmaceutical Sciences, Jilin University, Changchun, China. FAU - Wang, Chunling AU - Wang C AD - School of Pharmaceutical Sciences, Jilin University, Changchun, China. FAU - Wan, Hongle AU - Wan H AD - School of Pharmaceutical Sciences, Jilin University, Changchun, China; School of Pharmaceutical Sciences, Jiamusi University, Jiamusi, China. FAU - Li, Li AU - Li L AD - School of Pharmaceutical Sciences, Jilin University, Changchun, China. FAU - Zhang, Muxin AU - Zhang M AD - School of Pharmaceutical Sciences, Jilin University, Changchun, China. FAU - Zhang, Mengyuan AU - Zhang M AD - School of Pharmaceutical Sciences, Jilin University, Changchun, China. FAU - Zhang, Weidong AU - Zhang W AD - School of Pharmaceutical Sciences, Jilin University, Changchun, China. Electronic address: weidongzhang@jlu.edu.cn. LA - eng PT - Journal Article DEP - 20230705 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 2415-24-9 (catalpol) SB - IM MH - *Rehmannia MH - *Molecular Imprinting/methods MH - Microspheres MH - Adsorption MH - Magnetic Phenomena MH - Solid Phase Extraction/methods MH - Chromatography, High Pressure Liquid OTO - NOTNLM OT - Catalpol OT - Magnetic solid-phase extraction OT - Molecularly imprinted polymers OT - Rehmannia glutinosa COIS- Declaration of Competing Interest We declare that we have no financial and personal relationships with other people or organizations that can inappropriately influence our work. There is no professional or other personal interest of any nature or kind in any product, service and/or company that could be construed as influencing the position presented in, or the review of, the manuscript entitled. EDAT- 2023/07/16 19:16 MHDA- 2023/08/09 06:43 CRDT- 2023/07/16 18:02 PHST- 2023/03/23 00:00 [received] PHST- 2023/06/27 00:00 [revised] PHST- 2023/06/27 00:00 [accepted] PHST- 2023/08/09 06:43 [medline] PHST- 2023/07/16 19:16 [pubmed] PHST- 2023/07/16 18:02 [entrez] AID - S0021-9673(23)00409-0 [pii] AID - 10.1016/j.chroma.2023.464183 [doi] PST - ppublish SO - J Chromatogr A. 2023 Aug 30;1705:464183. doi: 10.1016/j.chroma.2023.464183. Epub 2023 Jul 5.