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以甲基丙烯酸二甲氨乙酯为单体,2-溴异丁酰溴为引发剂,CuBr/五甲基二乙烯基三胺(PMDETA)为催化剂,通过原子转移自由基聚合(ATRP)反应,将甲基丙烯酸二甲氨乙酯(DMAEMA)接枝到5μm大孔硅胶表面上,得到了接枝聚合物(PDMAEMA)亲水作用色谱固定相.通过改变反应体系中单体的量,制备了三种不同接枝量的亲水作用色谱固定相,利用元素分析对所制备的固定相进行了表征.详细考察了该固定相的分离性能以及流动相中盐浓度、水含量对溶质保留行为的影响,并将该固定相用于宁心宝胶囊中核苷类化合物的分离和测定.在亲水模式下,该固定相可以基线分离7种核苷类化合物,保留时间随着接枝量的增加而增大,与氨基亲水作用色谱柱相比,该合成柱的分离效率高,溶质在该填料上的保留符合分配作用保留机理.实验结果表明,该填料具有良好的分离性能.
ATRP reaction was carried out with dimethylaminoethyl methacrylate monomer, 2-bromoisobutyryl bromide as initiator and CuBr / pentamethyldivinylamine (PMDETA) as catalyst. (DMAEMA) was grafted onto the surface of 5μm macroporous silica gel to get the hydrophilic phase of the grafted polymer (PDMAEMA), which was prepared by changing the amount of monomer in the reaction system Three kinds of stationary phase of hydrophilic interaction chromatography with different grafting amount were characterized by elemental analysis.The separation performance of the stationary phase and the effect of salt concentration and water content on the retention of solute , And the stationary phase is used for the separation and determination of nucleoside compounds in Ningxinbao Capsules.In the hydrophilic mode, the stationary phase can separate seven nucleoside compounds at baseline, and the retention time varies with the grafting amount The separation efficiency of the column is higher than that of the hydrophilic amino group, and the retention of the solute on the packed column accords with the retention mechanism of the partitioning effect.The experimental results show that the column has good separation performance.