基于UPLC-LTQ-Orbitrap-MS的小儿扶脾颗粒的化学成分研究

Study on chemical constituents from Xiaoer Fupi Granules based on UPLC-LTQ-Orbitrap-MS

目的系统阐明中药复方小儿扶脾颗粒中的化学成分,建立一种对中药复方复杂成分快速鉴定的液质分析方法。方法采用超高效液相色谱-离子阱-静电场轨道阱质谱(UPLC-LTQ-Orbitrap-MS)对小儿扶脾颗粒成分进行分析,色谱柱为Waters HSS T3-C18色谱柱(100 mm×2.1 mm,1.8μm),流动相为0.1%甲酸水(A)-乙腈(B),梯度洗脱,体积流量0.3 mL/min。根据UPLC-LTQ-Orbitrap-MS扫描提供化合物的准确相对分子质量、多级质谱数据、质谱碎片离子信息等,参照对照品、文献报道等进行成分鉴定。结果共鉴定了小儿扶脾中颗粒共84个化学成分,主要包括黄酮类、糖苷类、酚酸及其酯类等,并对各成分的药材来源进行归属,同时根据质量规律和多级质谱裂解规律建立了快速鉴定黄酮类以及多甲氧基黄酮类化合物的方法。结论对小儿扶脾颗粒的化学成分进行了较为全面的分析,为其药效物质基础研究及质量控制提供了一定的理论依据。

Objective To clarify the chemical constituents from Xiaoer Fupi Granules and establish an effective identification method for the complex composition of Chinese material medica. Methods UPLC-LTQ-Orbitrap-MS was used to analyze the chemical constituents of Xiaoer Fupi Granules. The analysis was performed on Waters HSS T3-C18(100 mm × 2.1 mm, 1.8 μm). The mobile phase consisted of 0.1% ammonium formate(A)-acetonitrile(B), which was used for gradient elution, with the flow rate of 0.3 m L/min. This objective was achieved mainly depending on the information of the accurate mass and the multistage fragment ions obtained by UPLC-LTQ-Orbitrap-MS, comparing the mass spectrometric data of the standard substance and consulting the reference literatures. Results A total of 84 compounds were identified in this study, including the flavones, glycosidics, phenoliacids, and its esters, and so on, which were attributed the herbs source of each compound. Meanwhile, an effective and quickly identification method for the glycosides, flavonoids, and polyoxyflavonoids were established based on the law of multistage mass spectrometry. ConclusionThe comprehensive chemical constituents analysis of Xiaoer Fupi Granules will provide the scientific theory basis for the pharmacodyamic material basis and the quality control of this drug.