Key Laboratory of Combinatorial Biosynthesis and Drug Discovery, Wuhan University, Ministry of Education, and Wuhan University School of Pharmaceutical Sciences, Wuhan 430071, China.
Talanta. 2013 Jan 15;103:103-9. doi: 10.1016/j.talanta.2012.10.014. Epub 2012 Oct 11.
A novel berberine-imprinted polymer (MIP) monolith was prepared for extraction of berberine in aqueous medium. The MIP monolith was prepared inside a polypropylene micropipette tip by using dimethylsulfoxide as porogen, acrylamide (AA) as functional monomer and ethyleneglyol dimethacrylate (EGDMA) as cross-linker. Polymerization conditions were optimized and good permeability and selectivity was obtained when the ratio of berberine/AA/EGDMA was 1:5:30. Cross-reaction was also studied by three compounds (palmatine, coptisine, and jatrorrhizine) with similar structure. A molecularly imprinted micro solid-phase extraction (MI-μ-SPE) method was developed for selective extraction of berberine in aqueous solutions. Extraction parameters were investigated, such as sample pH value, sample flow rate, sample volume and elution solvent. By combining with HPLC/UV, MI-μ-SPE method showed a good linear range of 3-800 ng/mL with a low limit of detection limit of 1.0 ng/mL. The method was also applied for the pretreatment of berberine in human plasma and urine samples. The result showed that proteins and other biological matrix were successfully eliminated and berberine was selectively enriched. Recoveries were tested in plasma and urine samples, and calculated to be 90.6-103.2% with relative standard deviations less than 4.7%.
一种新型的小檗碱印迹聚合物（MIP）整体柱被制备用于在水介质中提取小檗碱。MIP 整体柱是在聚丙烯微量进样管内通过使用二甲基亚砜作为致孔剂、丙烯酰胺（AA）作为功能单体和乙二醇二甲基丙烯酸酯（EGDMA）作为交联剂制备的。优化了聚合条件，当小檗碱/AA/EGDMA 的比例为 1:5:30 时，得到了良好的渗透性和选择性。还通过三种具有相似结构的化合物（巴马汀、黄连碱和防己诺林碱）研究了交叉反应。建立了一种用于水溶液中小檗碱选择性提取的分子印迹微固相萃取（MI-μ-SPE）方法。研究了萃取参数，如样品 pH 值、样品流速、样品体积和洗脱溶剂。通过与 HPLC/UV 结合，MI-μ-SPE 方法在 3-800ng/mL 的范围内表现出良好的线性，检测限低至 1.0ng/mL。该方法还应用于人血浆和尿液中小檗碱的预处理。结果表明，成功去除了蛋白质和其他生物基质，并且小檗碱被选择性地富集。在血浆和尿液样品中进行了回收率测试，回收率为 90.6-103.2%，相对标准偏差小于 4.7%。
