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作 者:杨筱静[1] 赵波[1] 那可[1] 赵文杰 朱宝泉[1]
机构地区:[1]中国医药工业研究总院上海医药工业研究院,创新药物与制药工艺国家重点实验室,上海200040 [2]中国医药集团四川抗菌素研究所,四川成都610052
出 处:《中国医药工业杂志》2013年第8期754-760,共7页Chinese Journal of Pharmaceuticals
基 金:国家"重大新药创制"科技重大专项(20122X9301002003-004);国家863计划(2011AA090702)
摘 要:1403B是具有抗肿瘤功能的海洋生物活性物质,是1403C制备过程中的主要杂质。本文阐述了建立的1403B粗晶制备方法 ;以PS30-300为介质从1403B粗晶中分离纯化1403B,通过高效液相色谱对解吸溶剂的比例和解吸pH条件进行快速筛选,得到1403B分离纯化工艺为:用1%乙酸的30%乙醇溶解1403B粗晶上柱,用1%乙酸的55%乙醇解吸,流速为0.8 ml/min;获得的1403B峰纯度≥96%,收率≥95%。1403B is the major impurity from fermentation process of 1403C which is marine bioactive substance with antitumor effect. This research established a method for preparation of 1403B coarse crystal and separation of 1403B from 1403B coarse crystal on the carrier of PS30-300, respectively. Quick screenings of desorption ratio and pH were carried out by high performance liquid chromatography. The isolate process of 1403B was as follows: 30% ethanol with 1% acetic acid was used to dissolve 1403B coarse crystal and 55% ethanol with 1% HOAc was for desorption at a flow rate of 0.8 ml/min. The chromatographic purity of 1403B was above 96% and the yield was above 95 %.
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