Rao K V V Prasada, Rani A, Reddy A V Raghava, Bharathi C H, Dandala Ramesh, Naidu A
Department of Chemical Research, Aurobindo Pharma Research Centre, 313 Bachupally, Quthubullapur Mandal, Hyderabad 500072, India.
J Pharm Biomed Anal. 2007 Mar 12;43(4):1476-82. doi: 10.1016/j.jpba.2006.10.031. Epub 2006 Dec 15.
Three unknown impurities in Cefdinir bulk drug at levels below 0.2% (ranging from 0.05 to 0.2%) have been detected by high performance liquid chromatography (HPLC). These impurities were isolated from crude sample of Cefdinir using preparative HPLC. Based on the spectral data (NMR, IR and MS) the structures of these impurities were characterized as (6R, 7R)-7-[(z)-2-(2-aminothiazol-4-yl)-2-hydroxyiminoacetamido]-8-oxo-3-vinyl-5-thia-1-azabicyclo [4.2.0] oct-2-ene-2-carboxylic acid-5-oxide (I). (6R, 7R)-7-[(z)-2-(2-aminothiazol-4-yl)-2-hydroxyiminoacetamido]-8-oxo-3-vinyl-5-thia-1-azabi-cyclo [4.2.0] oct-3-ene-2-carboxylic acid (II). (6R, 7R)-7-[(z)-2-(2-aminothiazol-4-yl)-2-hydroxyiminoacetamido]-8-oxo-3-methyl-5-thia-1-azabicyclo-[4.2.0]oct-2-ene-2-carboxylic acid (III), respectively. The origin and structural elucidation of all impurities have been discussed.
通过高效液相色谱法（HPLC）检测到头孢地尼原料药中存在三种未知杂质，含量低于0.2%（范围为0.05%至0.2%）。使用制备型HPLC从头孢地尼粗品中分离出这些杂质。根据光谱数据（核磁共振、红外光谱和质谱），这些杂质的结构分别被鉴定为（6R，7R）-7-[(Z)-2-(2-氨基噻唑-4-基)-2-羟基亚氨基乙酰胺基]-8-氧代-3-乙烯基-5-硫杂-1-氮杂双环[4.2.0]辛-2-烯-2-羧酸-5-氧化物（I）、（6R，7R）-7-[(Z)-2-(2-氨基噻唑-4-基)-2-羟基亚氨基乙酰胺基]-8-氧代-3-乙烯基-5-硫杂-1-氮杂双环[4.2.0]辛-3-烯-2-羧酸（II）、（6R，7R）-7-[(Z)-2-(2-氨基噻唑-4-基)-2-羟基亚氨基乙酰胺基]-8-氧代-3-甲基-5-硫杂-1-氮杂双环[4.2.0]辛-2-烯-2-羧酸（III）。已对所有杂质的来源和结构解析进行了讨论。
Zotero 插件