摘要
在克拉霉素合成工艺中,红霉素肟的醚化保护是最重要的一步。作者研究确立了一种反相高效液相色谱法,能有效地对醚化产物红霉素A9 (1 异丙氧环己基)肟及其与工艺相关的化合物进行分离和定量分析。色谱柱为DIKMA公司的InertsilODS-3(150mm×4 6mm,粒径5μm)。流动相为V(乙腈)∶V〔c(KH2PO4)=0 033mol/L〕=48∶52,流速1 5mL/min,UV检测波长205nm,柱温30℃。肟醚在进样量为10～50μg内具有良好的线性关系,为醚化反应的工艺优化和监控提供了一个可在10min内快速而可靠的检测方法。作者还对红霉素A9 (1 异丙氧环己基)肟的E和Z异构体进行了定性分离和色谱行为研究,结果表明Z异构体比E的保留时间短,流动相V(乙腈)∶V〔c(KH2PO4)=0 033mol/L〕=45∶55时,分离度最好。
Erythromycin A 9(1isopropoxycyclohexyl) oxime is the key intermediate for the synthesis of clarithromycin.A quantitative reversedphase HPLC method for separation of this intermediate and related substances in the process using DIKMAInertsil ODS-3 column(150 mm×46 mm,5 μm) at 30 ℃ and CH3CN-0033 mol/L KH2PO4(V∶V=48∶52) as mobile phase with flow rate of 15 mL/min and UV 205 nm detector was established. In quick determination of the intermediate a good linearity was obtained in the range of 10-50 μg, r=09986 and RSD=0310%.At the same time the qualitative separation method for E and Zisomer of erythromycin A 9(1isopropoxycyclohexyl) oxime was investigated.The results showed that Zisomer had less retention time than Eisomer,and the best resolution of the isomers was obtained using CH3CN-0033 mol/L KH2PO4(V∶V=45∶55) as mobile phase.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2003年第4期254-256,共3页
Fine Chemicals
基金
国家经贸委技术创新项目(01BK-009)
