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氨溴索中一种降解产物的高效液相色谱联用技术分离、鉴定及表征

Isolation, Identification, and Characterization of One Degradation Product in Ambroxol by HPLC-Hyphenated Techniques.

作者信息

Thummala Veera Raghava Raju, Ivaturi Mrutyunjaya Rao, Nittala Someswara Rao

机构信息

Analytical Research and Development, Integrated Product Development, Dr. Reddy's Laboratories Ltd., Bachupally, Hyderabad-500 072, India.

School of Chemistry, Andhra University, Visakhapatnam-530003, A.P., India.

出版信息

Sci Pharm. 2014 Jan 12;82(2):247-63. doi: 10.3797/scipharm.1310-21. Print 2014 Apr-Jun.

DOI:10.3797/scipharm.1310-21
PMID:24959402
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC4065121/
Abstract

This study details the isolation, identification, and characterization of ambroxol's unknown impurity. One unknown impurity of ambroxol was formed in the formulated drug under stress conditions [40°C /75% relative humidity (RH) for 6 months] with the relative retention time (RRT) 0.68 in RP-HPLC. The impurity was enriched by exposing it to heat and it was isolated by using preparative HPLC. The enriched impurity was purified and characterized using the following sophisticated techniques: 2D NMR (gDQ-COSY, gHSQC, and gHMBC), FTIR, and LC-MS/MS. On the basis of the spectral data, the impurity was characterized as trans-4-(6,8-dibromoquinazolin-3(4H)-yl)cyclohexanol.

摘要

本研究详细阐述了氨溴索未知杂质的分离、鉴定及表征。在加速试验条件（40°C/75%相对湿度，6个月）下，氨溴索的一种未知杂质在制剂中形成，其在反相高效液相色谱中的相对保留时间（RRT）为0.68。该杂质经加热富集，并通过制备型高效液相色谱进行分离。采用二维核磁共振（gDQ-COSY、gHSQC和gHMBC）、傅里叶变换红外光谱（FTIR）以及液相色谱-串联质谱（LC-MS/MS）等精密技术对富集后的杂质进行纯化和表征。基于光谱数据，该杂质被鉴定为反式-4-(6,8-二溴喹唑啉-3(4H)-基)环己醇。

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本文引用的文献

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Determination of ambroxol hydrochloride, methylparaben and benzoic acid in pharmaceutical preparations based on sequential injection technique coupled with monolithic column.基于顺序注射技术与整体柱联用测定药物制剂中的盐酸氨溴索、对羟基苯甲酸甲酯和苯甲酸
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