分子印迹固相萃取/高效液相色谱法分离和富集枳实中4种黄烷酮

Molecularly Imprinted Solid-phase Extraction Combined with High Performance Liquid Chromatography for Separation and Enrichment of Four Flavanones in Citrus Aurantium

采用沉淀聚合法以橙皮素为模板分子,2-乙烯基吡啶为功能单体,二甲基丙烯酸乙二醇酯为交联剂,合成了橙皮素分子印迹聚合物。利用紫外光谱法确定了最佳功能单体与配比,优化了合成条件。采用傅立叶变换红外光谱、扫描电子显微镜、静态吸附对聚合物进行表征。实验结果表明,分子印迹聚合物的吸附性能明显优于空白印迹聚合物,且此聚合物对柚皮苷、橙皮苷、柚皮素和橙皮素的相对选择系数分别为1.40,1.39,1.59和2.89,表明该分子印迹聚合物对4种黄烷酮有较好的选择性。将印迹聚合物作为固相萃取填料,对枳实提取液进行分离和富集,结果表明上述4种黄烷酮的提取率分别为72.6%,61.1%,95.4%和93.5%,分离富集效果良好,大大提高了枳实中4种黄烷酮的提取效率。

A molecularly imprinted polymer to recognize four flavanones（hesperetin,hesperidin,naringenin,naringin） was prepared via precipitation polymerization using hesperetin as template molecule,2-vinylpyridine（2-VP） as functional monomer,and ethylene glycol dimethacrylate（EGDMA） as cross-linking agent. The optimal functional monomer and ratio were selected by UV spectrum method,and the optimized synthesis conditions were obtained. The molecularly imprinted polymer（MIP） and non-molecularly imprinted polymer（NIP） were characterized by scanning electron microscopy（SEM）,Fourier transform infrared spectroscopy（FTIR） and static adsorption experiments. The MIP and NIP were used as selective sorbents for the comparative determination of naringin,hesperidin,naringenin,hesperetin.The results showed that the MIP had higher selective adsorption capacity to four flavanones than the NIP,and the relative selectivity coefficients（Ie） were 1.40,1.39,1.59 and 2.89,respectively. A molecularly imprinted solid phase extraction（MISPE）column filled with the polymer material was prepared to enrich and separate four flavanones in Citrus aurantium.In the optimum conditions,four flavanones of the Citrus aurantium was extracted by solid phase extraction.The results showed that the extraction efficiencies for four flavanones were 72.6%（naringin）,61.1%（hesperidin）,95.4%（naringenin） and 93.5%（hesperetin）,respectively. The MISPE with neglectable matrix interference exhitited a good separation effect and greatly improved the extraction efficiencies for four flavanones in Citrus aurantium.