Shao Huikai, Zhao Lingguo, Chen Jian, Zhou Haitao, Huang Shuting, Li Kang
School of Pharmacy, Guangdong Pharmaceutical University, Guangzhou 510006, China.
Center for Disease Prevention and Control of Futian District, Shenzhen 518040, China.
J Pharm Biomed Anal. 2015;111:241-7. doi: 10.1016/j.jpba.2015.04.006. Epub 2015 Apr 8.
The molecularly imprinted solid-phase extraction (MISPE) monolithic column coupled with high-performance liquid chromatography (HPLC) was firstly developed for the extraction of hesperetin in the flesh of Citrus reticulata cv. Chachiensis, which is a traditional Chinese medicine (TCM). The molecularly imprinted polymers (MIPs) have been prepared by a thermal polymerization method using hesperetin as the template, acrylamide (AM) as functional monomer and ethylene glycol dimethacrylamide (EGDMA) as cross-linker in the mixed porogen of methanol, toluene and dodecanol. The prepared MIPs were characterized in detail by SEM and FTIR. The results confirmed the uniform and open structure of network skeleton with large flow-through pores. The influence of synthesis conditions on the specific recognition properties of hesperetin MIPs were also investigated systematically. The results showed that high adsorption capacity and good selectivity of MIPs were achieved when using non-imprinted polymer monolith (NIP) and structure similarly compound rutin as references. Furthermore, several parameters of the MISPE method have been optimized, and then it was successfully applied to the extraction of hesperetin from the flesh of Citrus reticulata cv. Chachiensis. Good gathering and impurity removing ability of prepared MIP were demonstrated. The MISPE method was proven to be a potentially competitive technique for separation and cleanup of hesperetin in complex TCM with satisfied recovery (90.8 ± 3.2%) and good precision (RSD = 6.48%).
首次开发了分子印迹固相萃取（MISPE）整体柱与高效液相色谱（HPLC）联用技术，用于提取中药化州橙果肉中的橙皮素。以橙皮素为模板，丙烯酰胺（AM）为功能单体，乙二醇二甲基丙烯酸酯（EGDMA）为交联剂，在甲醇、甲苯和十二醇的混合致孔剂中，通过热聚合法制备了分子印迹聚合物（MIPs）。采用扫描电子显微镜（SEM）和傅里叶变换红外光谱（FTIR）对制备的MIPs进行了详细表征。结果证实了其具有大通孔的均匀开放网络骨架结构。系统研究了合成条件对橙皮素MIPs特异性识别性能的影响。结果表明，以非印迹聚合物整体柱（NIP）和结构类似的化合物芦丁为参比时，MIPs具有高吸附容量和良好的选择性。此外，对MISPE方法的几个参数进行了优化，并成功应用于化州橙果肉中橙皮素的提取。结果表明，所制备的MIP具有良好的富集和去除杂质能力。MISPE方法被证明是一种在复杂中药中分离和净化橙皮素的潜在竞争技术，回收率令人满意（90.8±3.2%），精密度良好（RSD = 6.48%）。
