HPLC-Q-Exactive-MS/MS快速鉴定蒙药三子散化学成分

Rapid Identification of the Chemical Components of Mongolian Medicine Sanzi Powder by HPLC-Q-Exactive-MS/MS

关键词:  三子散  HPLC-Q-Exactive-MS/MS  化学成分

Key words:  Sanzi powder  HPLC-Q-exactive-MS/MS  chemical constituents

摘要:

目的 采用HPLC-Q-Exactive-MS/MS对三子散复方中化学成分进行快速定性分析。方法 SHIMADZU GIST C₁₈色谱柱(4.6 mm×150 mm，5 μm)，以0.1%甲酸水-甲醇为流动相，梯度洗脱，流速0.5 mL·min^-1，柱温30 ℃，正、负离子模式下扫描三子散的一级、二级质谱信息。以总离子流图分析的分子离子峰和碎片离子的质谱信息、分子式、保留时间，结合Chemspider数据库及参考文献查找的分子式和结构式，对三子散中各成分进行定性归属。结果 通过分析各类成分的质谱裂解规律和文献信息，初步推测出95个可能的化学成分，包括39个酚酸类成分、20个鞣质成分、9个有机酸酯类成分、5个单萜类成分、12个环烯醚萜类成分、8个三萜类成分和2个黄酮类成分。其中，57个来自诃子，30个来自栀子，10个来自川楝子，其中芦丁同时来源于诃子、栀子和川楝子。结论 HPLC-Q-Exactive-MS/MS检测方法分离度好、灵敏度高，可快速、高效地推测出三子散中各类成分，为鉴定三子散中的化学成分建立了一种快速、高效的分析方法。

Abstract:

OBJECTIVE To quickly qualitatively analyze the chemical components in Sanzi powder compound prescription by HPLC-Q-Exactive-MS/MS. METHODS SHIMADZU GIST C₁₈ column(4.6 mm×150 mm, 5 μm) was used, using 0.1% formic acid water-methanol as mobile phase with gradient elution, the flow rate was 0.5 mL·min^-1, the column temperature was 30 ℃. Under positive and negative ion modes, the primary and secondary mass spectrometry information of Sanzi powder was scanned. Qualitative attribution of each component in Sanzi powder was carried out based on the mass spectrometry information, molecular formula, and retention time of molecular ion peaks and fragment ions analyzed using total ion flow diagrams, combined with the molecular formula and structural formula searched in the Chemspider database and references. RESULTS Based on the analysis of the mass spectrometry cleavage rules and references of various components, 95 possible chemical components were preliminarily inferred, including 39 phenolic acids, 20 tannins, 9 organic acid esters, 5 monoterpenoids, 12 iridoids, 8 triterpenes and 2 flavonoids. Among them, 57 components were from Chebulae Fructus, 30 were from Gardeniae Fructus, 10 were from Toosendan Fructus, and among these compounds, rutin from Chebulae Fructus, Gardeniae Fructus and Toosendan Fructus. CONCLUSION The HPLC-Q-Exactive-MS/MS detection method has good separation and high sensitivity, and can quickly and efficiently infer various components in Sanzi powder. It establishes a fast and efficient analytical method for identifying the chemical components in Sanzi powder.