中国中药杂志

2018, v.43(14) 2872-2877

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UPLC-QTOF-MS鉴定注射用灯盏花素原料药中相关物质的结构
Structural identification of related substances in Breviscapine by UPLC-QTOF-MS

赵猛;王鹏飞;王晓梅;刘远;刘晓谦;陈两绵;高慧敏;王智民;张伟;
ZHAO Meng;WANG Peng-fei;WANG Xiao-mei;LIU Yuan;LIU Xiao-qian;CHEN Liang-mian;GAO Hui-min;WANG Zhi-min;ZHANG Wei;College of Pharmacy,Henan University of Chinese Medicine;National Engineering Laboratory for Quality Control Technology of Chinese Herbal Medicine,Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences;Tianjin University of Traditional Chinese Medicine;Kunming Longjin Pharmaceutical Co.,Ltd.;

摘要(Abstract):

为了系统明确注射用灯盏花素原料药相关物质组成,采用HPLC对不同厂家18批次原料药和灯盏花乙醇提取物以及灯盏花素精制母液浓缩物进行分析,利用UPLC-QTOF-MS对其中的相关物质进行结构鉴定。在选定的色谱条件下,灯盏乙素与相关物质能很好地分离,共检测出13个杂质峰,基于UPLC-QTOF-MS提供的精确相对分子质量、碎片离子特征,结合对照品,分别鉴定为6-羟基芹菜素-6-O-葡萄糖-7-O-葡萄糖醛酸苷(1),5,7,8,3',4',5'-六羟基黄酮-7-O-葡萄糖醛酸苷(2),5,6,7,3',4'-五羟基黄酮-7-O-葡萄糖醛酸苷(3)及其异构体(4),patuletin-3-O-葡萄糖醛酸苷(5),甲氧基灯盏乙素(6),灯盏甲素(7),异鼠李素-7-O-葡萄糖醛酸苷(8),香叶木素-7-O-葡萄糖醛酸苷(9),野黄芩素(10),灯盏乙素甲酯(11),灯盏乙素乙酯(12),芹菜素(13)。该研究明确了注射用灯盏花素原料药的相关物质,为改善原料药及其制剂的质量控制提供了参考依据。
To systematically identify the related substances in the original materials of breviscapine injection,18 batches of samples collected from different pharmaceutical companies,its ethanol extract and breviscapine mother liquor concentrate were analyzed by high performance liquid chromatography(HPLC),and their structures were identified by ultra performance liquid chromatography and quadruple/time-of-flight mass spectrometry(UPLC-QTOF-MS). Under the selected chromatographic conditions,scutellarin and related substances have good resolution and 13 related substances were observed. Based on the molecular weight and fragmentation patterns obtained by UPLC-QTOF-MS as well as reference substances,their structures were elucidated as 6-hydroxyapigenin-6-O-glucosyl-7-O-glucuronide(1),5,7,8,3',4',5'-hexahydroxyflavone-7-O-glucuronide(2),5,6,7,3',4'-pentahydroxyflavone-7-O-glucuronide(3) and its isomer(4),patuletin-3-O-glucuronide(5),methoxylscutellarin(6),apigenin 7-O-glucuronide(7),isorhamnetin 7-O-glucuronide(8),diosmetin 7-O-glucuronide(9),scutellarein(10),scutellarin methyl ester(11),scutellarin ethyl ester(12),and apigenin(13). This study has clarified related substances in the original materials of breviscapine injection,providing references for the improvement of quality control for breviscapine drug material and its preparations

关键词(KeyWords): 灯盏花素;相关物质;结构鉴定;HPLC;UPLC-QTOF-MS
breviscapine;related substance;structural identification;HPLC;UPLC-QTOF-MS

Abstract:

Keywords:

基金项目(Foundation): 国家中药标准化项目(ZYBZH-C-YN-59)

作者(Author): 赵猛;王鹏飞;王晓梅;刘远;刘晓谦;陈两绵;高慧敏;王智民;张伟;
ZHAO Meng;WANG Peng-fei;WANG Xiao-mei;LIU Yuan;LIU Xiao-qian;CHEN Liang-mian;GAO Hui-min;WANG Zhi-min;ZHANG Wei;College of Pharmacy,Henan University of Chinese Medicine;National Engineering Laboratory for Quality Control Technology of Chinese Herbal Medicine,Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences;Tianjin University of Traditional Chinese Medicine;Kunming Longjin Pharmaceutical Co.,Ltd.;

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