| 引用本文: | 王伟,喻承昊,谭艳云,潘远江.泊沙康唑新异构体杂质分离纯化及其结构表征[J].中国现代应用药学,2024,41(20):110-116. |
| WANG Wei,YU Chenghao,TAN Yanyun,PAN Yuanjiang.Separation and characterization of new isomer in posaconazole[J].Chin J Mod Appl Pharm(中国现代应用药学),2024,41(20):110-116. |
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| 摘要: |
| 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×20mm，10μm），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。 |
| 关键词: 泊沙康唑 异构体杂质 结构表征 |
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| Separation and characterization of new isomer in posaconazole |
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WANG Wei1, YU Chenghao2, TAN Yanyun2, PAN Yuanjiang3
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1.杭州泽邦科技有限公司;2.Hangzhou Zebon Technology Co., Ltd,;3.Zhejiang University
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| Abstract: |
| OBJECTIVE To separate and identify the chemical structure of new isomer in posaconazole. METHODS The novel isomer of posaconazole was isolated and purified by semi-preparative HPLC. Luna C18(2) (250 mm×20mm, 10μm) column was used, and the mixture of acetonitrile-water containing 0.1% v/v 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. |
| Key words: posaconazole isomer structural characterization |
