UPLC-ESI-Q-TOF-MS在分析山茱萸化学成分中的应用

Application of UPLC-ESI-Q-TOF-MS on Chemical Constitutents of Cornus officinalis

关键词:  山茱萸  水溶性成分  醇溶性成分  超高效液相色谱电喷雾四极杆飞行时间串联质谱  碰撞诱导解离

Key words:  Cornus officinalis  water-soluble constitutents  alcohol-soluble constitutents  UPLC-ESI-Q-TOF-MS  CID

摘要:

目的 采用超高效液相色谱电喷雾四级杆飞行时间串联质谱(UPLC-ESI-Q-TOF-MS)对山茱萸中水溶性成分以及醇溶性成分进行分析和鉴别。方法 用ACQUITY UPLC HSS T3 C₁₈柱(2.1 mm×100 mm，1.8 mm)，以0.2%甲酸水溶液-0.2%甲酸甲醇溶液为流动相梯度洗脱；使用ESI离子源，分别在正离子和负离子模式下采集数据。结果 推断出山茱萸水溶性成分5种：没食子酸，莫罗忍冬苷，马钱素，山茱萸新苷Ⅰ，当药苷；醇溶性成分5种：7-脱氢马钱素，山茱萸新苷Ⅱ，槲皮素，齐墩果酸，熊果酸。结论 经过超高效液相色谱的分离，借助Q-TOF-MS测定得到的精确分子质量及正负离子信息可以鉴定山茱萸中水溶性成分和醇溶性成分，为其成分鉴定提供了一种准确有效的方法。

Abstract:

OBJECTIVE To analyze and identify water-soluble composition and alcohol-soluble composition in Cornus officinalis. METHODS These constituents were determined by UPLC-ESI-Q-TOF-MS. The chromatographic separation was performed on ACQUITY UPLC HSS T3 C₁₈ (2.1 mm×100 mm, 1.8 μm) with a gradient elution of water containing 0.2% formic acid-methanol containing 0.2% formic acid. The mass spectrometer equipped with electrospray ionization source was used as a detector. And data was collected under the positive and negative ion modes. RESULTS Five water-soluble constituents were identified as gallic acid, morroniside, loganin, cornuside Ⅰ, sweroside. And five alcohol-soluble constituents were identified as 7-dehydrologanin, cornuside Ⅱ, quercetin, oleanolic acid, ursolic acid. CONCLUSION In this study, water-soluble and alcohol-soluble constitutents in Cornus officinalis were separated by UPLC, and identified through the information of positive ion and negative ion and accurate MW(molecular weight) which were determined by UPLC-ESI-Q-TOF-MS. It is an accurate and effective method which can be applied for the constituent identification of Cornus officinalis.