Ultra-performance LC separation and quadrupole time-of-flight MS identification of major alkaloids in Plumula Nelumbinis.
Ultra-performance LC separation and quadrupole time-of-flight MS identification of major alkaloids in Plumula Nelumbinis.
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DOI：
10.1002/pca.2517
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发表时间：
2014-11
期刊：
影响因子：
--
通讯作者：
Li W
中科院分区：
文献类型：
--
作者：
Lin Z;Yang R;Guan Z;Chen A;Li W
莲蓬作为许多国家的重要药物和茶叶来源，其主要生物活性可能通过其生物碱发挥。然而，由于缺乏对其化学成分的研究，其活性尚未完全了解。建立超高效液相色谱-二极管阵列检测器（UPLC-DAD）结合电喷雾电离-四极杆飞行时间质谱（ESI-QTof MS）分离鉴定白乳香生物碱的方法。采用高效液相色谱法（UPLC）分离蓝冠草乙醇提取物，将洗脱液直接注入ESI-QTof质谱系统。采用低碰撞能（CE）和高碰撞能（CE）的ESI正离子模式和负离子模式来获得足够的质谱信息。根据其色谱特征、紫外光谱、精确质量、质谱片段和文献报道初步鉴定了21种生物碱。它们由6种双-1-苄基四氢异喹啉、11种苄基四氢异喹啉（含2种糖生物碱和2种季铵）、2种阿波啡、1种原阿波啡和1种吲哚生物碱组成。其中11个为首次鉴定，7个为首次报道。对5个化合物进行了表征，分别为：去甲氯尿-4′- o -葡萄糖苷、去甲氯尿-6- o -葡萄糖苷、异糖氨酸、6-去甲基-4′-甲基-n -甲基氯尿和n -去甲异亮氨酸。所建立的UPLC-DAD-ESI-QTof-MS方法可有效地对莲叶提取物中的生物碱进行系统鉴定。
As an essential medicine and tea source in many countries, Plumula Nelumbinis potentially exerts its major biological activities through its alkaloids. However, its activities are not fully understood due to the lack of studies on its chemical components. To establish an Ultra Performance Liquid Chromatography–Diode-Array Detector (UPLC–DAD) method, combined with an Electrospray Ionization–Quadrupole Time-of-flight Mass Spectrometry (ESI–QTof MS), for the separation and identification of Plumula Nelumbinis alkaloids. The eluant from an UPLC separation of an ethanol extract of Plumula Nelumbinis was directly infused into an ESI–QTof MS system. Both positive and negative ion modes of ESI with low and high Collision Energy (CE) were used to obtain sufficient MS information. 21 alkaloids were tentatively identified based on their chromatographic characteristics, UV spectra, exact mass, MS fragments, and literature reports. They consist of 6 bis-1-benzyltetrahydroisoquinoline, 11 benzyltetrahydroisoquinoline (containing 2 glycoalkaloids and 2 quaternary ammoniums), 2 aporphine, one proaporphine, and one indole alkaloids. Eleven were identified in Plumula Nelumbinis for the first time and 7 were firstly reported in Nelumbo nucifera Gaertn. Five compounds, namely norcoclaurine-4′-O-glucoside, norcoclaurine-6-O-glucoside, isolotusine, 6-demethyl-4′-methyl-N-methylcoclaurine and N-norisoliensinine, were characterized and proposed as new compounds. The established UPLC–DAD–ESI–QTof–MS method is efficient for systematic identification of the alkaloids in Plumula Nelumbinis extract.