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 %.
出处
《中国医药工业杂志》
CAS
CSCD
北大核心
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)