药学学报, 2019, 54(9): 1655-1660
引用本文:
王静静, 堵伟锋, 卫星红, 谢子立, 程杰. 替硝唑葡萄糖注射液杂质的色谱-质谱结构鉴定[J]. 药学学报, 2019, 54(9): 1655-1660.
WANG Jing-jing, DU Wei-feng, WEI Xing-hong, XIE Zi-li, CHENG Jie. Identification of impurity profile in tinidazole glucose injection by UPLC-MS[J]. Acta Pharmaceutica Sinica, 2019, 54(9): 1655-1660.

替硝唑葡萄糖注射液杂质的色谱-质谱结构鉴定
王静静1, 堵伟锋2, 卫星红2, 谢子立2, 程杰2
1. 安徽中医药大学, 安徽 合肥 230038;
2. 安徽省食品药品检验研究院, 安徽 合肥 230051
摘要:
本文采用UPLC-Q Exactive四极杆-静电场轨道阱高分辨液质联用技术,结合对照品保留时间定位、有机反应理论、紫外光谱等手段检测并鉴定了替硝唑葡萄糖注射液杂质谱中的5个杂质,分别为2-甲基-5-硝基咪唑(杂质1)、5-羟甲基糠醛(杂质2)、1-(2-乙基磺酰基-乙基)-2-甲基-4-硝基-1H-咪唑(杂质5)、1-[2-(乙硫氧基)乙基]-2-甲基-5-硝基-1H-咪唑(杂质6)和1,4-二-N-氧代-2-甲基-5-硝基-1H-咪唑(杂质8),其中杂质6和杂质8为首次报道。该研究为替硝唑葡萄糖注射液的工艺优化和质量控制提供了参考依据。
关键词:    替硝唑葡萄糖注射液      有机杂质      色谱-质谱联用      结构鉴定     
Identification of impurity profile in tinidazole glucose injection by UPLC-MS
WANG Jing-jing1, DU Wei-feng2, WEI Xing-hong2, XIE Zi-li2, CHENG Jie2
1. Anhui University of Chinese Medicine, Hefei 230038, China;
2. Anhui Institute for Food and Drug Control, Hefei 230051, China
Abstract:
Five components in the impurity profile of tinidazole glucose injection were detected and identified by UPLC-Q Exactive quadrupole-electrostatic field orbitrap high resolution mass spectrometry, in combination with retention time references, organic reaction mechanisms and UV spectral analysis. They are 2-methyl-5-nitroimidazole (impurity 1), 5-hydroxymethylfurfural (impurity 2), 1-(2-(ethylsulfonyl)ethyl)-2-methyl-4-nitro-1H-Imidazole (impurity 5), 1-(2-(ethylthio)ethyl)-2-methyl-5-nitro-1H-imidazole (impurity 6) and 1,4-di-N-oxo-2-methyl-5-nitro-1H-imidazole (impurity 8) respectively, of which impurities 6 and 8 are identified for the first time. These results and detection methods are useful for monitoring the manufacturing process and quality control of tinidazole and glucose injection solution.
Key words:    tinidazole and glucose injection    organic impurity    UPLC-MS    structure identification   
收稿日期: 2019-04-12
DOI: 10.16438/j.0513-4870.2019-0278
基金项目: 2018年国家药品计划抽检品种1号.
通讯作者: 谢子立,Tel:86-551-63358051,E-mail:1536838165@qq.com;程杰,Tel:86-551-63358051,E-mail:chengjie_234@163.com
Email: 1536838165@qq.com;chengjie_234@163.com
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