摘要
为降低林可霉素B组分,本研究考察了高效液相制备色谱处理盐酸林可霉素工段中盐酸反萃液的工艺。通过对填料的筛选,上样液pH、上样量及洗脱条件的考察,确定了最终的色谱纯化工艺:LK-1为填料,上样液pH8.0,上样量10%,1倍柱体积水洗除组分B,3倍柱体积丙酮解析组分A。将丙酮解析液用盐酸调至pH2,结晶析出产品。纯化后,样品中B组分含量由约3%降低至0.5%以下。色谱分离收率大于90%,分离周期小于1h,该工艺应用于生产可高效地降低林可霉素B组分。
In order to lower the content of lincomycin B component, purification by preparative high performance liquid chromatography (HPLC) was studied. In this study, the hydrochloric acid extract of lincomycin was separated. The final chromatographic purification process was determined by screening packings, pH of sample solution, sample loading and elution conditions. LK-1 was selected as packing with pH 8.0 of sample solution and 10% of sample loading (weight). 1-Fold column volume of water and 3-fold column volume of acetone were used to elute the component B and the targeted component A, respectively. Preparative separation was carried out on 50DAC. The elution of acetone was modified to pH 2, and then the product was precipitated(crystallization yield was 91%). After purification, the content of lincomycin B decreased from about 3% to less than 0.5%.The recovery rate of lincomycin A was 92.7% and the purity of product was 98.94%. With short separation period(<1 h), this novel process can be efficiently used to lower the content of lincomycin B in manufacture.
作者
吴海波
薛兴亚
李奎永
周永正
WU Haibo;XUE Xingya;LI Kuiyong;ZHOU Yongzheng(Zhejiang Acchrom Technologines Co.,Ltd.,Wenling 317503;Key Lab.of Separation Science for Analytical Chemistry,Dalian Institute of Chemical Physics,Chinese Academy of Sciences,Dalian 116023)
出处
《中国医药工业杂志》
CAS
CSCD
北大核心
2019年第9期976-980,共5页
Chinese Journal of Pharmaceuticals
关键词
林可霉素A
林可霉素B
纯化
高效液相制备色谱
工艺改进
lincomycin A
lincomycin B
purification
high performance preparative liquid chromatography
improved process
