藏药诃子化学成分的高效液相色谱-质谱联用技术快速鉴定研究

Study on Rapid Identification of Constituents of Tibetan Medicine Terminalia chebular Retz. by HPLC/LTQ-Orbitrap MS^n

目的:建立高效液相色谱-线性离子阱/静电场轨道阱组合式高分辨质谱联用(HPLC-LTQ-Orbitrap MS)技术分析藏药诃子化学成分的方法。方法:采用Diamonsil C18色谱柱(4.6 mm×250 mm,5μm),以甲醇-0.2%乙酸水为流动相进行梯度洗脱。在负离子模式下,采集LTQ-Orbitrap线性离子阱高分辨质谱数据,依据高分辨质谱提供的分子离子峰和碎片离子的精确分子质量,并与文献或对照品对照,确定化合物可能的结构。结果:从诃子中鉴定出62种化学成分,包括酚酸类和可水解鞣质类60个,三萜类2个,其中,14个化合物在该植物中首次检出。结论:该方法可为诃子的化学成分质谱裂解规律和质量控制提供参考。

The aim of this work was to identify and analyze the chemical constituents of Terminalia chebular Retz by establishing high performance liquid chromatography-linear ion trap/electrostatic field orbitrap combined high resolution mass spectrometry(HPLC-LTQ-Orbitrap MS) technique. With the application of C18 reverse phase column(4.6 mm×250 mm, 5 μm), gradient elution was performed with methanol and water(0.2% acetic acid) as mobile phase.In negative ionization mode, the data of LTQ-Orbitrap was collected. Accurate molecular mass of molecular ion peaks and fragment ions provided by the high-resolution mass spectrometry were compared with the literature and the reference substance to determine the possible structure of the compound. The results indicated that 62 compounds from the extract of Terminalia chebular Retz. were identified, including acids and hydrolysable tannins(60), triterpenoids(2). There were14 compounds were detected from this specie for the first time. It is proved as an effective method to provide reference for Chemical composition mass spectrometry and the quality control in further phytochemical studies of Terminalia chebular Retz.