Jubilant Life Sciences Ltd., Analytical Research Department, R&D Centre, C-26, Sector-59, Noida 201301, Uttar Pradesh, India. saji
J Pharm Biomed Anal. 2011 Sep 10;56(2):423-8. doi: 10.1016/j.jpba.2011.05.030. Epub 2011 May 27.
Two impurities were detected in the HPLC analysis of crude carbamazepine active pharmaceutical ingredient. One of the impurities of the order of 0.5% was found to be unknown and has not been reported previously. A LC-MS compatible reverse phase isocratic method was developed and tandem mass spectrometry was performed using electrospray ionization source and ion trap mass analyzer. Isolation of unknown impurity was performed by semi-preparative HPLC followed by characterization using nuclear magnetic resonance spectroscopy (NMR), infrared spectroscopy (FT-IR) and elemental analysis (CHNS) confirmed its structure as tetrabenzo[b,f,b'f']azepino[4',5':4,5]thieno[2,3-d]azepine-3,9-dicarboxamide. A plausible mechanism for the formation of this impurity is proposed.
在粗制卡马西平原料药的 HPLC 分析中检测到两种杂质。其中一种杂质的含量约为 0.5%，为未知杂质，此前尚未有报道。开发了一种与 LC-MS 兼容的反相等度方法，并使用电喷雾电离源和离子阱质谱分析仪进行串联质谱分析。通过半制备 HPLC 对未知杂质进行分离，然后使用核磁共振波谱（NMR）、红外光谱（FT-IR）和元素分析（CHNS）进行表征，确认其结构为四苯并[b,f,b'f']氮杂卓[4',5':4,5]噻吩并[2,3-d]氮杂卓-3,9-二羧酸酰胺。提出了该杂质形成的可能机制。
