State Key Laboratory of Chemo/Biosensing and Chemometrics, College of Chemistry and Chemical Engineering, Hunan University, Changsha, PR China.
Analyst. 2011 Feb 21;136(4):756-63. doi: 10.1039/c0an00798f. Epub 2010 Dec 13.
In the present work, an improved and direct approach for the preparation of molecularly imprinted polymers (MIPs) was proposed. The MIPs were prepared based on bulk polymerization by water-bath heating and ultrasonic elution of the template, using rutin as the template, acrylamide (AM) as the functional monomer and 2,2'-azobisisobutyronitrile (AIBN) as the cross linker. Molecularly imprinted polymers prepared by other elution methods, including microwave-assisted extraction and conventional Soxhlet extraction, were used for comparison and the results showed that the ultrasonic elution method is the best. The synthesized MIPs were characterized by Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). High performance liquid chromatography (HPLC) was used to evaluate the adsorption properties and recognition mechanism of the MIPs. Structurally similar compounds including quercetin and genistein were utilized for verifying the molecular selectivity and characterizing the recognition capability of the MIPs. The MIPs were used as a sorbent for the solid phase extraction of rutin, and the resultant cartridge showed a good extraction performance. Thus, a molecularly imprinted solid-phase extraction (MISPE) procedure for selective pre-concentration of rutin from complicated traditional Chinese medicine (TCM) samples was proposed. Various elution parameters that affect the adsorption capacity of the polymer were evaluated to optimize the selective pre-concentration of rutin. The characteristics of the MISPE method were validated by HPLC. The recoveries ranged from 85% to 91% for TCMs, which demonstrated that this MISPE-HPLC method could be applied to pre-concentrate and determinate rutin directly from complicated TCM samples in the presence of other interfering substances.
在本工作中,提出了一种改进的、直接的分子印迹聚合物(MIP)制备方法。通过水浴加热和模板超声洗脱的本体聚合方法,以芦丁为模板、丙烯酰胺(AM)为功能单体、2,2'-偶氮二异丁腈(AIBN)为交联剂,制备了分子印迹聚合物。采用其他洗脱方法(包括微波辅助萃取和常规索氏提取)制备的分子印迹聚合物进行了比较,结果表明超声洗脱法最佳。采用傅里叶变换红外(FT-IR)光谱和扫描电子显微镜(SEM)对合成的 MIP 进行了表征。高效液相色谱(HPLC)用于评价 MIP 的吸附性能和识别机制。利用结构类似的化合物槲皮素和染料木黄酮验证了 MIP 的分子选择性,并表征了其识别能力。将 MIP 用作芦丁固相萃取的吸附剂,所得萃取柱具有良好的萃取性能。因此,提出了一种用于从复杂中药(TCM)样品中选择性预浓缩芦丁的分子印迹固相萃取(MISPE)方法。评估了各种洗脱参数对聚合物吸附容量的影响,以优化芦丁的选择性预浓缩。采用 HPLC 验证了 MISPE 方法的特点。对于 TCM,回收率在 85%至 91%之间,表明该 MISPE-HPLC 方法可用于在存在其他干扰物质的情况下,直接从复杂的 TCM 样品中预浓缩和测定芦丁。