首页|泊沙康唑新异构体杂质分离纯化及其结构表征

泊沙康唑新异构体杂质分离纯化及其结构表征

扫码查看
目的 对泊沙康唑新发现的同分异构体杂质进行分离纯化及其结构表征。方法 采用半制备液相色谱,色谱柱为Luna C18(2)(250 mm×20 mm,10 μm),乙腈-0。1%甲酸水为流动相进行分离纯化,成功制备了一个新异构体杂质纯品,利用高效液相色谱质谱联用法与核磁共振波谱法快速鉴定异构体杂质。结果 泊沙康唑新异构体杂质被鉴定为4-(4-(4-(4-(((3R,5R)-5-((1H-1,2,4-三唑-1-基)甲基)-5-(2,4-二氟苯基)四氢呋喃-3-基)甲氧基)苯基)哌嗪-1-基)苯基)-1-((2S,3S)-2-羟基戊基-2-基)-1H-1,2,4-三唑-5(4H)-酮),该杂质为首次鉴定的新化合物。结论 泊沙康唑的新异构体杂质分离纯化及结构确证对该产品的质量控制具有重要意义。
Isolation,Purification and Structural Characterization of New Isomer in Posaconazole
OBJECTIVE To isolation,purify and identify the chemical structure of new isomer in posaconazole.METHODS The novel isomer of posaconazole was isolated and purified by semi-preparative HPLC,and the column was Luna C18(2)(250 mm× 20 mm,10 μm),and the mixture of acetonitrile-water containing 0.1%formic acid was used as mobile phase and the pure new isomer was successfully obtained.The isomer was quickly identified by LC-MS and NMR techniques.RESULTS The novel isomer was identified as 4-(4-(4-(4-(((3R,5R)-5-((1H-1,2,4-triazol-1-yl)methyl)-5-(2,4-difluorophenyl)tetrahydrofuran-3-yl)methoxy)phenyl)piperazin-1-yl)phenyl)-1-((2S,3S)-2-hydroxypentan-2-yl)-1H-1,2,4-triazol-5(4H)-one,and it was identified for the first time.CONCLUSION The separation and structural characterization of posaconazole isomer is of great significance to the quality control of posaconazole.

posaconazoleisomerstructural characterization

王伟、喻承昊、谭艳云、潘远江

展开 >

杭州泽邦科技有限公司,杭州 310000

浙江大学化学系,杭州 310058

泊沙康唑 异构体杂质 结构表征

2024

中国现代应用药学
中国药学会

中国现代应用药学

CSTPCD北大核心
影响因子:0.877
ISSN:1007-7693
年,卷(期):2024.41(20)