去羟肌苷中新杂质的鉴定与表征

Identification and characterization of new impurity in didanosine.

作者信息

Srinivasa Rao D V N, Srinivas N, Bharathi Ch, Prasad Ch S, Dandala Ramesh, Naidu A

机构信息

Department of Chemical Research, Aurobindo Pharma Research Centre, 313 Bachupally, Quthubullapur Mandal, Hyderabad 500072, India.

出版信息

J Pharm Biomed Anal. 2007 Nov 5;45(3):516-20. doi: 10.1016/j.jpba.2007.05.034. Epub 2007 Jun 3.

DOI:10.1016/j.jpba.2007.05.034

PMID:17624711

Abstract

Didanosine is an antiviral drug. During the preparation of didanosine in our lab, six process related known impurities and one unknown impurity were detected in HPLC analysis at levels ranging from 0.05 to 0.8%. The same unknown impurity was also observed in commercial batches. This new impurity was isolated by preparative HPLC and co-injected with didanosine sample to confirm the retention times in HPLC. This impurity was characterized as, 9-(2,3,5-trideoxy-beta-D-glycero-pentofuranosyl)-9H-purin-6-one (2',3',5'-trideoxyinosine). Structural elucidation of this impurity by spectral data (1H NMR, 13C NMR, MS and IR) has been discussed.

摘要

去羟肌苷是一种抗病毒药物。在我们实验室制备去羟肌苷的过程中，高效液相色谱（HPLC）分析检测到六种与工艺相关的已知杂质和一种未知杂质，含量范围为0.05%至0.8%。在市售批次中也观察到了相同的未知杂质。通过制备型HPLC分离出这种新杂质，并与去羟肌苷样品共注入以确认其在HPLC中的保留时间。该杂质被鉴定为9-(2,3,5-三脱氧-β-D-甘油-戊呋喃糖基)-9H-嘌呤-6-酮（2',3',5'-三脱氧肌苷）。已讨论通过光谱数据（1H NMR、13C NMR、MS和IR）对该杂质进行结构解析。