| 李辉,王素素,张月,李志平.化学通报,2015,78(8):738-743. |
| 绿原酸印迹均匀微球的制备及其色谱行为研究 |
| Investigation on preparation and chromatographic behavior of monodisperse chlorogenic acid imprinted polymers |
| 投稿时间：2014-12-15 修订日期：2015-01-04 |
| DOI： |
| 中文关键词: 分子印迹微球 沉淀聚合 绿原酸 色谱行为 |
| 英文关键词:Molecularly imprinted polymer microspheres Precipitation polymerization Chromatographic behavior |
| 基金项目:国家自然科学基金项目 |
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| 中文摘要: |
| 以绿原酸为模板,甲基丙烯酸为功能单体,二乙烯基苯为交联剂,采用沉淀聚合法制备了绿原酸印迹均匀微球。探讨了模板及功能单体类型和用量对聚合物颗粒均匀性的影响,考察了流动相组成及柱温对分子印迹柱色谱保留和选择性的影响。绿原酸均匀印迹微球的制备条件为：模板-功能单体-交联剂的用量比为0.375:1.5:7.0,摇瓶转速为15r/min时,微球直径约2.5μm,聚合物收率为35.4%。流动相组成及含水量对印迹聚合物的保留行为影响较大,当用乙腈-水混合物为流动相时,含水量增加,各化合物在印迹色谱柱上的容量因子降低：当流动相含水量高于2.5%,分子印迹聚合物失去选择识别能力；但以0.002mol L-1磷酸缓冲液(pH3.0)-乙腈混合液为流动相时,分子印迹柱对模板的容量因子、选择性及色谱峰形都有较大改进。当二者体积比为19:1,容量因子高达90.69,其选择性相对于没食子酸和原儿茶酸高达23.10和6.562。温度影响分子印迹聚合物的选择保留能力,当温度从25℃提高到45℃时,印迹聚合物对模板的容量因子从3.52降低到2.41,选择因子降低约30%。 |
| 英文摘要: |
| A homogeneous chlorogenic acid imprinted polymers (MIPs) microsphere was prepared by precipitation polymerization technique using methacrylic acid (MAA) and divinylbenzene (DVB) as functional monomer and cross-linker, respectively. The influence of template and functional monomer type and volume on particle size uniformity was discussed and that of mobile phase composition and column temperature on retention behavior and selectivity of the MIPs column explored. These uniform imprinted microspheres (2.5μm particle size ) were obtained under the conditions of molar ratio 0.375:1.5:7.0 of template-functional monomer-cross linker at the rotate speed 15r/min of flask, with a yield of 35.4%. The mobile phase composition and water-containing volume affected the retention of the template on the MIPs column. Capacity factors of the MIPs decreased with water-containing ratio when acetonitrile-water mixture was used as mobile phase and no selectivity could be observed at higher than 2.5% water-containing percentage in acetonitrile. However, using mobile phase consisting of 0.002 mol L-1 phosphoric acid buffer (pH 3.0)-acitonitrile mixture could improve the capacity factor, selectivity and chromatographic peak shape. When the volume ratio of two solvents was at 19:1, the capacity factor of the MIPs column was the highest, with a value of 90.69 and the selectivity of this column toward the template relative to gallic acid and protocatechuic acid reached 23.10 and 6.562, respectively. In addition, temperature could affect retention of the MIPs column and the capacity factors decreased from 3.52 to 2.41, with a 30% decrease in selectivity when temperature was increased from 25 to 45℃. |
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