硅醚化制备克拉霉素中相关杂质的色谱分离与检验  

Chromatographic Separation and Identification of Related Impurities in Preparation of Clarithromycin through Reaction of Silyl-Etherification

作　　者：冯玉玲[1] 孙京国[1] 

机构地区：[1]河北师范大学化学与材料科学学院,石家庄050016

出　　处：《中国现代应用药学》2009年第3期234-236,共3页Chinese Journal of Modern Applied Pharmacy

基　　金：河北省教育厅科研基金资助项目(Z2005210);河北师范大学博士基金(L2003B12)

摘　　要：目的分离和确证硅醚化法制备克拉霉素的相关杂质。方法先用TLC找杂质分离条件,再用柱色谱分离提纯,建立HPLC分析方法,以1H-NMR和MALDI-TOF-MS确证结构。结果用色谱和波谱得到并确证了相关杂质分别为4″-O-三甲基硅红霉素A肟(4)和4″-O-三甲基硅红霉素A9(O-叔丁基二甲基硅)肟(5)。结论色谱方法适合于克拉霉素制备中的硅醚化监控。OBJECTIVE Separation and identification of related impurities in preparation of clarithromycin through reaction of silyl-etherification. METHODS The separation condition of impurities was optimized by TLC at first, Separation and purification of the related impurities were conducted by column chromatograph. HPLC chromatograph condition was established. The related impurities in the silyl-etherification were idertified by using ^1H-NMR and MALDI-TOF-MS. RESULTS The related impurities were confirmed as 4″ -O-trimethylsilyl erythromycin A oxime （ 4 ） and 4″ -O-trimethylsilyl erythromycin A 9 （ o-t-butyldimethylsilyl ） oxime （ 5 ） by chromatography and spectroscopy. CONCLUSION The method could efficiently controll and monitor the quality of clarithromycin preparation in the silyl-etherification procedure.

关 键 词：克拉霉素 硅醚 杂质 色谱 鉴定 

分 类 号：R917.101[医药卫生—药物分析学] TQ465.5[医药卫生—药学]