pH区带逆流色谱法制备高纯度ATP竞争性mTOR抑制剂AZD2014  

Preparation of High Purity ATP-competitive mTOR Inhibitor AZD2014 by pH-zone Refining Counter-current Chromatography

作　　者：杨国新[1] 陈夏琴[1] 陈晓明[1] 余辉[1] 程元荣[1] 黄捷[1] YANG Guo-xin;CHEN Xia-qin;CHEN Xiao-ming;YU Hui;CHENG Yuan-rong;HUANG Jie(Fujian Institute of Microbiology,Fuzhou 350007,China)

机构地区：[1]福建省微生物研究所,福州350007

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)

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.

关 键 词：pH区带逆流色谱 AZD2014 分离纯化 

分 类 号：R94[医药卫生—药剂学]