基于UPLC-Q―TOF―MS-MS技术快速探析淫羊藿总黄酮胶囊中化学成分.docVIP

基于UPLC/Q―TOF―MS/MS技术快速探析淫羊藿总黄酮胶囊中化学成分 　　[摘要] 应用超高效液相色谱-四极杆飞行时间质谱联用技术（UPLC/Q-TOF-MS/MS），对淫羊藿总黄酮胶囊的化学成分进行分析和鉴定，采用Agilent SB-C18色谱柱 （2.1 mm×100 mm，1.8 μm），以0.1%甲酸水溶液和乙腈为流动相，梯度洗脱，体积流速0.3 mLmin-1，柱温30 ℃，进样量2 μL。质谱采用电喷雾（ESI）离子源，正负离子模式下采集数据，根据精确相对分子质量，二级质谱裂解碎片和色谱峰保留时间等信息结合对照品的碎片裂解规律和文献数据进行结构鉴定。结果共鉴定或推测出46个化合物，包括黄酮苷类、酚酸类以及生物碱类化合物。该结果为淫羊藿总黄酮胶囊的质量控制、后期临床应用提供了技术支持，并为进一步阐明其药效物质基础提供参考 [关键词] 淫羊藿总黄酮胶囊；UPLC/Q-TOF-MS/MS；黄酮苷；酚酸；生物碱 [Abstract] To analyze and identify the chemical constituents from Yinyanghuo Zonghuangtong capsule by using UPLC/Q-TOF-MS/MS. Chromatographic separation was carried out on an Agilent SB-C18 column （2.1 mm×100 mm，1.8 μm） at the temperature of 30 ℃. The mobile phase was 0.1% formic acid and acetonitrile by gradient elution，with a flow rate at 0.30 mLmin-1，and the injection volume of 2 μL. The MS spectrum was acquired in both negative and positive ion modes using ESI ion source. Based on relative accurate molecular weight，secondary mass spectrometry pyrolysis fragments and chromatographic peak retention time，as well as fragmentation regularity summarized from reference substance and the literature，we could effectively identify the chemical structure of the components under test. As a result，a total of 46 compounds，including flavonoid glycosides，phenolic acids and alkaloids，were successfully identified or tentatively predicted. The results provide technical support for quality control and late-stage clinical application of Yinyanghuo Zonghuangtong capsule，and reference for further expound the pharmacodynamic material basis. [Key words] Yinyanghuo Zonghuangtong capsule；UPLC/Q-TOF-MS/MS；flavonoid glycosides；phenolic acids；alkaloids doi：10.4268/cjcm 淫羊藿?黄酮胶囊由小檗科植物淫羊藿Epimedium brevicornu Maxim.的总黄酮提取物制成，具有温补肾阳、强筋健骨的功效，于2014年获得新药证书，临床用于原发性骨质疏松症肾阳虚证。总黄酮作为淫羊藿的主要活性成分，具有广泛的药理作用，如壮阳，抗骨质疏松，保护神经系统，促进免疫系统，抗癌等[1-5]，是最具开发潜力的中药有效部位之一。目前，针对淫羊藿药材化学成分分析的相关研究已有不少报道[6-8]，且不同品种的淫羊藿所含化学成分相差较大，而针对淫羊藿总黄酮胶囊全面的化学成分分析还未见报道，物质基础的不明确一定程度上限制了其质量控制及药效物质基础的深入研究。鉴于淫羊藿不同品