纽莫康定杂质C_(0)的制备研究  

Study on the preparation of pneumocandin C_(0)

作　　者：曾凡洲 刘志钰 朱兵峰 王钦超 张贵民 魏荣省 Zeng Fan-zhou;Liu Zhi-yu;Zhu Bing-feng;Wang Qin-chao;Zhang Gui-min;Wei Rong-sheng(Lunan New Time Bio-Tech Co.,Ltd.,Linyi 273400;Lunan Pharmaceutical Group Co.,Ltd.,Linyi 273400;National Engineering Laboratory for High-level Expression in Mammalian Cells,Linyi 273400)

机构地区：[1]鲁南新时代生物技术有限公司,临沂273400 [2]鲁南制药集团股份有限公司,临沂273400 [3]哺乳动物细胞高效表达国家工程实验室,临沂273400

出　　处：《中国抗生素杂志》2022年第3期280-288,共9页Chinese Journal of Antibiotics

摘　　要：目的 为控制纽莫康定B_(0)的质量及为卡泊芬净的杂质传递研究提供物料,本研究对关键杂质纽莫康定C_(0)进行了制备。方法 通过发酵液提取工艺富集、高压液相制备色谱、减压浓缩、冷冻干燥,制备得到纽莫康定C_(0)干粉,并对其进行紫外吸收光谱、红外吸收光谱、核磁共振、质谱等分析和结构鉴定。结果 得到了色谱纯度99.19%、峰纯度999.4(DAD检测器)、热重3.05%的纽莫康定C_(0)干粉1.7395 g,其结构经过确证为纽莫康定C_(0)。结论 制备得到的纽莫康定C_(0),可作为质量研究对照品和杂质传递研究用物料,并对纽莫康定其他杂质的制备具有重要参考价值。Objective In order to control the quality of pneumocandin B_(0)and provide materials for impurity transfer research of caspofungin, pneumocandin C_(0)was prepared as the key impurity. Methods Through the enrichment of fermentation broth extraction process, high pressure liquid chromatography, vacuum concentration, and freeze-drying, the objective impurity was prepared. Its structure was analyzed and identified by ultraviolet absorption spectroscopy, infrared absorption spectroscopy, nuclear magnetic resonance, and mass spectrometry. Results 1.7395 g freeze-dried powder with chromatographic purity of 99.19 %, DAD peak purity of 999.4 and thermogravimetry of 3.05% was obtained. Its structure was confirmed as peomocondin C_(0). Conclusion The powder could be used as the reference substance for quality research and materials for impurity transfer research. This study is of considerable referential value for preparation of other peomocondin-related impurities.

关 键 词：纽莫康定C_(0)制备 高压液相制备色谱 结构确证 

分 类 号：TQ463[化学工程—制药化工]