尼麦角林有关物质的色谱质谱结构鉴定Identificationof-药学学报.PDF

1026 药学学报 Acta Pharmaceutica Sinica 20 15, 50 (8): 1026 1031 麦角林有关物质的色谱 质谱结构鉴定 1 2 1 1* 曾雪芳 , 刘 洁 , 宋 敏 , 杭太俊 (1. 中国药科大学, 江苏 南京 210009; 2. 海南省食品药品检验所, 海南 海口 570100) 摘要: 为了研究尼麦角林及其制剂中的有关物质, 采用电喷雾正离子化 飞行时间质谱法 (ESI-TOF/MS) 测 定各有关物质的准确质量, 三重四极质谱 (ESI-MS/MS) 测定子离子特征。根据对照品比对、质谱裂解分析, 结 合合成工艺与强制降解实验, 检测并鉴定了尼麦角林及其制剂中的 16 个主要有关物质 (8 个合成副产物、8 个降 解产物), 为尼麦角林生产工艺控制和质量保障提供参考依据。 关键词: 尼麦角林; 有关物质; 色谱 质谱联用; 裂解规律 中图分类号: R9 17 文献标识码: A 文章编号: 0513-4870 (20 15) 08- 1026-06 Identification of related substances in nicergoline by HPLC-MS 1 2 1 1* ZENG Xue-fang , LIU Jie , SONG Min , HANG Tai-jun (1. China Pharmaceutical University, Nanj ing 210009, China; 2. Hainan Provincial Institutefo r Drug and Food Control, Haikou 5 70100, China ) Abstract : To study the related substances in nicergoline, electrospray positive ionization high resolution TOF/MS was used for the determination of the accurate mass and elemental composition of the related substances. Triple quadrupoles tandem MS/MS was employed for the determination of the fragmentations of the parent ions. 16 related substances were detected and identified to be eight synthetic by-products and eight degradation products, by using impurity references matching, product mass spectra fragmentations elucidation, and verified further according to synthetic processes and stress testing results. The results obtained are valuable for nicergoline manufacturin