灯心草及野灯心草中菲类成分的LCESIMS快速识别及鉴定.pdfVIP

中草药 Chinese Traditional and Herbal Drugs 第 44 卷 第 12 期 2013 年 6 月 ·1539 · 灯心草及野灯心草中菲类成分的 LC-ESI-MS 快速识别及鉴定 赵丹丹，李贵云，王小红，王 杨，林宏英，黄建梅* 北京中医药大学中药学院，北京 100102 摘 要：目的 快速识别及鉴定灯心草及野灯心草中的菲类成分。方法 运用高效液相色谱- 电喷雾质谱（HPLC-ESI-MS ） 联用技术研究菲类成分的裂解规律，并分别对灯心草和野灯心草甲醇提取液中的菲类成分进行快速识别和鉴定。结果 在负 离子模式下，菲类成分容易丢失 2H 的碎片，推测可能是乙烯基与苯环环合而失去2 个氢；也易发生重排丢失羰基，呈现出 一定的裂解规律。根据菲类成分的裂解规律，从灯心草和野灯心草甲醇提取物中快速筛选了 21 个菲类成分，其中 6 个成分 经与对照品比对而准确鉴定；另外结合质谱裂解信息及极性差异，推测出其中 5 个成分的结构。结论 HPLC-ESI-MS 技术 既可以从中药复杂体系中快速识别菲类成分并根据裂解规律初步确定菲类成分结构，也是实现中药中目标天然产物定向分离 的有效手段。 关键词：灯心草；野灯心草；菲类；高效液相色谱- 电喷雾质谱；质谱裂解 中图分类号：R284.1 文献标志码：A 文章编号：0253 - 2670(2013)12 - 1539 - 07 DOI: 10.7501/j.issn.0253-2670.2013.12.004 Rapid recognition and identification of phenanthrenes in Juncus effusus and Juncus setchuensis by LC-ESI-MS ZHAO Dan-dan, LI Gui-yun, WANG Xiao-hong, WANG Yang, LIN Hong-ying, HUANG Jian-mei School of Chinese Materia Medica, Beijing University of Chinese Medicine, Beijing 100102, China Abstract: Objective To rapidly recognize and identify phenanthrenes in Juncus effusus and J. setchuensis. Methods HPLC-ESI- MS method was used to investigate the ESI-MS characteristics of those phenanthrenes, to screen, and to identify phenanthrenes in J. effusus and J. setchuensis. Results Under negative mode, phenanthrenes were inclined to loss two hydrogens, which presumably caused by the cyclization of vinyl and aromatic ring; Furthermore, the loss of C=O could be also observed. Fragmentation pathway of phenanthrenes in ESI as a negative ion mode was summarized. Twenty-one phenanthrenes were rapidly detected from the extracts of J. effusus and J. setchuensis. Among them, six compounds were accurately identified by comparison with reference substances; The structures of five compounds were inferred according to their MS spectrum and polarity. Conclusion HPLC-ESI-MS provides not only a new technique for the rapid identification of phenanthrenes