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投稿时间:2016-12-15
投稿时间:2016-12-15
中文摘要: 采用大孔吸附树脂与阳离子交换树脂串联纯化四角蛤蜊醇沉上清液中核苷类成分,以核苷的纯度和回收率为指标,考察树脂的型号、上样浓度、水洗体积、洗脱剂浓度及流速对纯化效果的影响,以期得到最佳的纯化工艺。确定大孔吸附树脂的型号及最佳工艺为:SP207型,质量浓度250 mg/mL,pH值为5.0,水洗除杂体积是3 BV,洗脱液为体积分数5%乙醇。进一步通过离子交换树脂纯化,确定树脂型号及最佳纯化工艺为:001*7阳离子交换树脂,质量浓度6.3 mg/mL,氨水∶乙醇(体积比3∶30)溶液洗脱,洗脱流速是3 BV/h。经两种树脂串联纯化后,四角蛤蜊醇沉上清液中核苷类成分的质量分数由1.80%提高至50.60%,总回收率为70.32%。工艺验证结果表明SP207大孔吸附树脂与001*7阳离子交换树脂串联纯化核苷类成分的方法稳定可行,能够用于四角蛤蜊核苷类成分的分离纯化。
Abstract:The nucleosides were purified by macroporous adsorption resin and cation exchange resin from Mactra veneriformis,the purity and recovery rate of nucleosides were determined.The influence of the resin model,sample concentration,washing volume,concentration and flow rate on the purification efficiency were investigated in order to obtain the best purification process.The type and optimum process of macroporous resin was SP207,sample concentration was 250 mg/mL,pH value was 5.0,removal of impurities with water was 3 BV,and the eluent was the ethanol of 5%volume fraction.While the further purification of ion exchange resin determined that the resin type and the best purification process was to use 001*7 cation exchange resin,sample concentration was 6.3 mg/mL,elution solution was prepared with ammonia,ethanol and water(the volume ratio was 3∶30),elution flow rate was 3 BV/h.After tandem and purification of the two resins,the nucleosides in the alcohol precipitation supernatant of mactra quadrangularis were increased from 1.80%to 50.6%,with a total recovery of 70.32%.The process validation showed that the way to use SP207 macroporous resin and 001*7 cation exchange resin to purify nucleosides was stable and feasible,which could be adopted in the separation and purification of nucleosides in Mactra veneriformis.
文章编号:201718007 中图分类号: 文献标志码:A
基金项目:国家公益性行业专项基金(201305007、201405017);国家高技术研究发展计划(863计划);江苏省高校优势学科建设工程项目(PAPD);江苏省青蓝工程(2016)
作者 | 单位 |
张倩1,2,刘睿1,2,3,程建明1,2,3,王欣之1,2,3,杜俊潮1,2,张文英1,2,吴皓1,2,3,* | 1.南京中医药大学药学院,江苏南京210023;2.江苏省海洋药用生物资源研究与开发重点实验室,江苏南京210023;3.江苏省中药资源产业化过程协同创新中心/中药资源产业化与方剂创新药物国家地方联合工程研究中心,江苏南京210023 |
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