摘要
目的应用pH区带逆流色谱制备高纯度ATP竞争性mTOR抑制剂AZD2014。方法以甲基叔丁基醚-正丁醇-甲醇-水(5∶4∶1∶10)为溶剂体系,上相加入氨水(20mmol·L^(-1))为固定相,下相加入盐酸(20mmol·L^(-1))为流动相,主机转速810r·min^(-1),流动相流速1. 5mL·min^(-1),检测波长为230nm。结果从250mg AZD2014样品中经一次分离可得到HPLC纯度为99. 89%的高纯度AZD2014纯品182mg。结论 pH区带逆流色谱能有效、快速制备高纯度的AZD2014。
OBJECTIVE To prepare high purity ATP-competitive mTOR inhibitor AZD2014 by pH-zone refining counter-current chromatography. METHODS The two phase solvent system was composed of methyl tert-butyl ether,n-butanol,methanol and water at a volume ratio of 5∶ 4∶ 1∶ 10,in which ammonium hydroxide was added to the organic stationary phase at 20 mmol·L-1 as a retainer,and hydrochloric acid was added to the lower stationary phase at 20 mmol·L-1 as an eluter. The separation was performed using the lower phase as the mobile phase at a flow rate of 1. 5 mL·min-1,revolution speed of 810 r·min-1 and detection wavelength of 230 nm. RESULTS From 250 mg of sample,182 mg of AZD2014 with purity of 99. 89% was obtained. CONCLUSION The pH-zone refining counter-current chromatography can effectively separate and prepare high purity AZD2014.
作者
杨国新
陈夏琴
陈晓明
余辉
程元荣
黄捷
YANG Guo-xin;CHEN Xia-qin;CHEN Xiao-ming;YU Hui;CHENG Yuan-rong;HUANG Jie(Fujian Institute of Microbiology,Fuzhou 350007,China)
出处
《海峡药学》
2018年第11期16-18,共3页
Strait Pharmaceutical Journal
基金
福建省科技计划项目(2015R1009-9)
福建省科技计划项目(2016R1009-9)
关键词
pH区带逆流色谱
AZD2014
分离纯化
pH-zone refining counter-current chromatography
AZD2014
Separation and purification
