基于整体材料的固相萃取与毛细管电泳技术联合分离检测桑叶中的多酚类物质

采用甲基丙烯酸丁酯(BMA)为单体、乙二醇二甲基丙烯酸酯(EDMA)为交联剂,合成了聚甲基丙烯酸丁酯-乙二醇二甲基丙烯酸酯(poly(BMA-co-EDMA))整体柱,并将其作为固相萃取整体柱与毛细管电泳联用,建立了桑叶中芦丁、绿原酸、槲皮素等多酚物质的分离检测方法。考察了固相萃取条件如淋洗液种类、淋洗液流速和体积、洗脱液种类对萃取效率的影响,并采用毛细管电泳进行分离分析。结果显示,芦丁、绿原酸、槲皮素均在10~160μg/mL范围内线性关系良好,相关系数分别为0.9955、0.9985、0.9995,检出限分别为4.65、1.12、3.49μg/mL,相对标准偏差分别为2.4%、0.98%、2.8%,平均回收率分别为94.7%、98.9%、102%。该固相萃取柱能有效富集和纯化桑叶中3种多酚物质。方法简便、快速、灵敏,适用于桑叶中3种多酚类物质的分离分析。

Separation and Determination of Polyphenols in Mulberry Leaves by Combination of Monolithic Materials based Solid Phase Extraction and Capillary Electrophoresis

A capillary electrophoresis with monolithic column solid phase extraction was established for the separation and detection of polyphenols such as rutin,chlorogenic acid and quercetin in mulberry leaves.The polybutyl methacrylate-ethylene glycol dimethacrylate(poly(BMA-co-EDMA)) monolithic column was synthesized by using butyl methacrylate(BMA) as monomer and ethylene glycol dimethacrylate(EDMA) as crosslinker.Effects of solid phase extraction conditions such as leacheate type,flow rate and volume of leacheate,eluent type on extraction efficiency were investigated,and the separation and analysis of three polyphenols were performed by capillary electrophoresis.Under the optimized conditions,there were good linear relationships for rutin,chlorogenic acid and quercetin in the range of 10-160 μg/mL with correlation coefficients of 0.995 5,0.998 5 and 0.999 5,respectively.The detection limits for rutin,chlorogenic acid and quercetin were 4.65,1.12,3.49 μg/mL,respectively.The average recoveries for three analytes were 94.7 %,98.9 % and 102 %,with relative standard deviations of 2.4 %,0.98 % and 2.8 %,respectively.Results showed that the solid phase extraction column could be used for the effective enrichment and purification of three polyphenols in mulberry leaves.The method is simple,rapid and sensitive,and is suitable for the separation and analysis of three polyphenols in mulberry leaves.