基于HPLC-Q-TOF-MS/MS的广枣果肉化学成分分析

目的 采用高效液相色谱-四级杆-飞行时间串联质谱(HPLC-Q-TOF-MS/MS)法对广枣醇提物的主要化学成分进行分析鉴定。方法 采用回流提取法制备广枣醇提物,以Agilent TC-C18(4.6 mm×250 mm,5 μm)柱为分析柱,并以0.2%甲酸-甲醇溶液为流动相,流速0.7 mL/min,柱温30℃,进样量25 μL,进行梯度洗脱;质谱采用电喷雾离子源,毛细管电压4.0 kV,干燥器流速10.0 L/min,干燥器温度350℃,雾化器压力35.0 psi(1 psi=6 894.8 Pa),正负离子模式下扫描采集数据,并对各主要色谱峰进行归属。结果 通过正负离子质谱信息及元素组成分析,并结合相关文献和对照品数据对照,共鉴定出42种化合物,主要为氨基酸类、有机酸类及黄酮类,其中首次在广枣中发现的成分有17种。结论 HPLC-Q-TOF-MS/MS兼具色谱的高分离特性和质谱的高灵敏度双重优势,能对广枣的主要化学成分进行定性分析,可为广枣药效物质的基础研究提供依据。
Objective To apply high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (HPLC-Q-TOF-MS/MS) method in analyzing and identifying the main components in the ethanol extract of Choerospondiatis fructus. Methods The ethanol extract of Choerospondiatis fructus was prepared by the refluxing methods, and the main components in the extracts were separated by the gradient elution method with Agilent TC-C18 column (250 mm×4.6 mm, 5 μm), methanol-0.2% formic acid as the mobile phase, at flow rate 0.7 mL/min, column temperature 30℃, and sample volume 25 μL. Mass spectrometry was applied for the qualitative analysis under the positive and negative ion modes and ESI ion source was used for mass spectra, Vcap 4.0 kV, drying gas 10 L/min, gas temperature 350℃, and nebulizer 35 psi (1 psi=6 894.8 Pa). The main chromatographic peaks were assigned by Q-TOF. Results Forty-two compounds were identified through direct comparison of both positive and negative ion mass data, the element composition analysis, the data of the literature and the information from reference substances, including amino acids, organic acids, and flavonoids. Among them 17 constituents have been firstly found in Choerospondiatis fructus. Conclusion HPLC-Q-TOF-MS/MS has the advantage of the efficient separation ability of HPLC and highly sensitive detection of MS, and is capable of making a qualitative analysis of the main components in Choerospondiatis fructus, which provides an evidence for study