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为开发从酶反应液中分离纯化5-氟尿苷的方法,研究了利用阴离子交换树脂以及硅胶柱色谱实现转化产物分离纯化的工艺;实验采用HPLC为检测方法,以5-氟尿苷含量为考察指标,从吸附量,洗脱率,回收率的角度考察了各种条件的影响。最终确定以D301树脂为吸附剂;最佳吸附条件为动态吸附,温度25℃,pH 8;动态洗脱,洗脱剂5%NaCl溶液,体积流量为3BV/h;再利用硅胶柱色谱,采用200～300目硅胶,以正己烷∶乙酸乙酯=12∶88作为洗脱剂,洗脱后结晶可得到5-氟尿苷纯品,色谱纯,最终收率72.4%。
In order to develop a method for the separation and purification of 5-fluorouridine from enzyme reaction solution, the separation and purification of conversion products by anion exchange resin and silica gel column chromatography were studied. The HPLC method was used as the detection method, The indexes were investigated, and the influence of various conditions was investigated from the viewpoints of adsorption amount, elution rate and recovery rate. The optimum adsorption conditions were dynamic adsorption, temperature 25 ℃, pH 8; dynamic elution, eluant 5% NaCl solution, volume flow rate 3BV / h; re-use of silica gel column chromatography, using 200 ~ 300 mesh silica gel, n-hexane: ethyl acetate = 12: 88 as eluent, eluted and crystallized to give pure 5-fluorouridine product, chromatographic purity, the final yield of 72.4%.