摘要
在相同的实验条件下,分别合成了以咖啡酸为模板的印迹分子聚合物和无模板分子聚合物。使用场发射扫描电镜法和吸附实验表征这两种聚合物材料的孔状结构和选择性吸附性能。然后利用印迹分子聚合物、无模板分子聚合物、C18萃取小柱这3种材料结合固相萃取法纯化山楂提取物中的咖啡酸,提取率分别为3.46、1.01、1.17μg/g。为了优化固相萃取过程,实验研究了不同洗脱剂的影响。分别利用用氯化胆碱和甘油、氯化胆碱和尿素(摩尔比均为1∶2)合成出两种低共熔溶剂。甲醇与这两种低共熔溶剂分别以不同的体积比混合作为洗脱剂,用于优化咖啡酸的固相萃取过程。实验结果表明,印迹分子聚合物是一种良好的固相萃取材料;当甲醇和甘油基低共熔溶剂在体积比为3∶1混合时,表现出最好的洗脱能力,得到咖啡酸的回收率为82.32%。
Molecularly imprinted polymers (MIPs) with caffeic acid as template and non-imprinted polymers (NIPs) materials were prepared in the same procedure. Field emission scanning electron microscopy (FE- SEM) and adsorption capacity test were used to evaluate characteristic of the new materials. MIPs, NIPs and C18 were used for rapid purification of caffeic acid from hawthorn with solid-phase extraction ( SPE ), and extract yields of caffeic acid with the proposed materials were 3.46 μg/g, 1. 01 μg/g and 1. 17 μg/g, respec- tively. To optimize the MIPs-SPE procedures, different kinds of elution solutions were studied. Deep eutectic solvents (DESs) were prepared by choline chloride (ChCl)-glycerol ( 1/2, n/n) and choline chloride-urea ( I/ 2, n/n). Methanol was mixed with the two kinds of DESs ( glycerol-based DESs, urea-based DESs) in different ratios (0.5:1, 1:1, 2:1, 3:1, 4:1, 5:1, v/v), and they were used to investigated as elution solutions in the above MIPs-SPE procedures. The results showed that MIPs were potential SPE materials, and methanol/ glycerol-based DESs ( 3 : 1, v/v) had the best elution capability with the recovery of 82.32%.
出处
《色谱》
CAS
CSCD
北大核心
2015年第8期792-798,共7页
Chinese Journal of Chromatography
基金
supported by Tianjin Municipal Natural Science Foundation of China(13JCYBJC42200)
Tianjin Municipal“131”Talents Program
关键词
固相萃取法
低共熔溶剂
印迹分子聚合物
咖啡酸
山楂
solid-phase extraction (SPE)
deep eutectic solvents
molecularly imprinted polymers (MIPs)
caffeic acid
hawthorn