UPLC-Q-TOF-MS/MS鉴定小儿清咽颗粒化学成分

Identification of Chemical Constituents in Xiao'er Qingyan Granules by UPLC-Q-TOF-MS/MS

关键词:  小儿清咽颗粒  超高效液相色谱-四极杆-飞行时间串联质谱法  化学成分  裂解规律

Key words:  Xiao'er Qingyan granules  UPLC-Q-TOF-MS/MS  chemical constituents  fragmentation pathway

摘要:

目的 基于超高效液相色谱-四极杆-飞行时间串联质谱(UPLC-Q-TOF-MS/MS)技术鉴定小儿清咽颗粒中的化学成分。方法 采用Phenomenex Kinetex XB C₁₈色谱柱(2.1 mm×150 mm，1.7 μm)，以0.1%甲酸水-乙腈为流动相体系，梯度洗脱，流速0.25 mL·min^–1，质谱采用电喷雾(ESI)离子源，以正、负离子模式采集多级质谱碎片信息。结果 通过高分辨质谱数据分析，结合参考文献数据以及对照品确认，共鉴别出59个化学成分，包括5个环烯醚萜类，15个有机酸类，5个色原酮类，14个黄酮类，4个木脂素类，9个苯乙醇苷类，2个核苷类，2个酚类及3个其他类，并对化合物的药材来源进行了归属。结论 本研究建立的分析方法灵敏、高效，可应用于小儿清咽颗粒各类化学成分的鉴定分析，为研究小儿清咽颗粒药效物质基础和作用机制提供重要依据。

Abstract:

OBJECTIVE To identify the chemical constituents of Xiao'er Qingyan granules by using UPLC-Q-TOF-MS technology.METHODS The separation was performed on a Phenomenex Kinetex XB C₁₈ column(2.1 mm×150 mm, 1.7 μm) with mobile phase of water(containing 0.1% formic acid)-acetonitrile with gradient elution at a flow rate of 0.25 mL·min^-1. Electrospray ion(ESI) source was applied to collect multi-level mass spectrometry fragment information under positive and negative ion modes. RESULTS A total of 59 chemical constituents were identified by high mass spectrometry data analysis, literature comparison and reference confirmation. The chemical constituent cluster was composed of 5 iridoids, 15 organic acids, 5 chromones, 14 flavonoids, 4 lignans, 9 phenylethanoid glycosides, 2 nucleosides, 2 phenols and 3 other compounds. Furthermore, all of the constituents were surveyed and classified according to their medicinal materials derivation. CONCLUSION The proposed method is sensitive and efficient, and can be applied in identification analysis of various chemical constituents of Xiao'er Qingyan granules, which provides a crucial basis for further studying the material of Xiao'er Qingyan granules' efficacy and mechanism.