Characterization of an unknown impurity in doxofylline using LC-MS and NMR

被引：3
作者：
Zhu, Peixi [1 ,2 ,3 ]
Lu, Jingxian [3 ]
Hong, Liya [3 ]
Su, Weike [1 ]
Van Schepdael, Ann [2 ]
Adams, Erwin [2 ]
机构：
[1] Zhejiang Univ Technol, Coll Pharmaceut Sci, Hangzhou 310014, Zhejiang, Peoples R China
[2] Univ Leuven, KU Leuven, Dept Pharmaceut & Pharmacol Sci, Pharmaceut Anal, Herestr 49,O&N2,PB 923, B-3000 Leuven, Belgium
[3] Zhejiang Inst Food & Drug Control, Hangzhou 310053, Zhejiang, Peoples R China
来源：
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS | 2017年 / 140卷
关键词：
Doxofylline; Impurity; LC-MS; NMR; C-13; H-1;
D O I：
10.1016/j.jpba.2017.03.025
中图分类号：
O65 [分析化学];
学科分类号：
070302 ; 081704 ;
摘要：
During quality control of doxofylline, a novel impurity was detected, which was above the identification threshold defined by ICH. First, a liquid chromatographic method compatible with mass spectrometric (MS) detection was developed. Based on tandem multistage MS and high resolution MS data, the unknown impurity was found to consist of two theophylline groups connected by a methylene group. The structure was further confirmed by 1D and 2D nuclear magnetic resonance (NMR) experiments after semi-preparative isolation. In addition, the formation of the impurity was also discussed. (C) 2017 Elsevier B.V. All rights reserved.
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收藏
页码：31 / 37
页数：7
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