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以樟柳碱(ASD)为模板分子,甲基丙烯酸(MAA)为功能单体,三羟甲基丙烷三甲基丙烯酸酯(TRIM)为交联剂,乙腈为致孔剂,采用沉淀聚合法,合成了对4种托烷类生物碱(樟柳碱、东莨菪碱、山莨菪碱、阿托品)具有类特异性识别能力的聚合物。通过紫外光谱预测法筛选了最佳功能单体与配比。采用振荡平衡吸附实验对印迹和非印迹聚合物进行了吸附性能表征,结果表明,印迹聚合物对4种生物碱的饱和吸附量分别为7.53,10.90,24.27,11.04μg/mg,相对选择性系数分别为3.58,1.49,1.62,2.25。以该分子印迹聚合物为固相萃取柱填料,采用分子印迹固相萃取/高效液相色谱法实现了藏药马尿泡中4种托烷类生物碱的高效富集和快速分离。该方法在2~250μg/m L范围内具有较好的线性关系,相关系数(r2)为0.999 9,检出限为0.26~0.39μg/m L,在10,50,100μg/g加标浓度下的平均回收率为70.0%~96.3%,相对标准偏差(RSD)≤5.7%。该固相萃取柱重复使用率高,分离效果良好,有效去除了样品中杂质的干扰,大大提高了马尿泡果实中4种托烷类生物碱的萃取效率。
Using anisodine (ASD) as template molecule, methacrylic acid (MAA) as functional monomer, trimethylolpropane trimethacrylate (TRIM) as crosslinking agent and acetonitrile as porogen, , A polymer that has class-specific recognition ability for four kinds of tropane alkaloids (anisodine, scopolamine, anisodamine, atropine) was synthesized. The best functional monomer and ratio were screened by ultraviolet spectrum prediction. The equilibrium adsorption experiments were used to characterize the adsorption properties of the imprinted and non-imprinted polymers. The results showed that the saturated adsorption capacities of the imprinted polymers on the four alkaloids were 7.53,10.90,24.27,11.04μg / mg, respectively. The relative selectivity coefficient Respectively 3.58,1.49,1.62,2.25. The molecularly imprinted polymers were used as solid-phase extraction (SPE) column packing, and the high-efficiency enrichment and rapid separation of four tropane alkaloids in Tibetan mareblasts were achieved by molecularly imprinted solid-phase extraction / high performance liquid chromatography. The method has a good linearity in the range of 2 ~ 250μg / m L with a correlation coefficient (r2) of 0.999 9 and a detection limit of 0.26 ~ 0.39μg / m L at 10,50,100μg / g spiked concentration The average recovery was 70.0% ~ 96.3% with relative standard deviation (RSD) ≤ 5.7%. The solid phase extraction column with high reusability, good separation effect, effectively remove the interference of impurities in the sample, greatly improving the horse urinary fruit 4 kinds of tropane alkaloids extraction efficiency.