目的 采用UPLC-Q-TOF-MS/MS技术解析九味熄风颗粒化学成分并建立5种酚酸类成分（天麻素、巴利森苷E、巴利森苷B、巴利森苷C、巴利森苷A）一测多评（ QAMS）定量测定方法。方法 应用Waters UPLC HSS T₃色谱柱，以甲醇-0.1%甲酸水为流动相洗脱梯度，体积流量0.3 mL·min^-1，柱温35℃，采用电喷雾离子源（ ESI），正、负离子模式扫描，根据质谱数据结合文献报道进行成分鉴定。采用Phenomenex Luna C₁₈色谱柱，乙腈-0.1%磷酸水为流动相梯度洗脱，体积流量1.0 mL·min^-1，柱温30℃，检测波长220 nm，以天麻素为内参物，建立其与4种酚类成分的相对校正因子，计算各待测组分的含量，比较外标法（ ESM）和QAMS这2种方法的差异。结果 从九味熄风颗粒中共推断和鉴定出92个化学成分，包括20个生物碱类、20个有机酸及其酯类、12个环烯醚萜类、6个酚类、6个氨基酸类、6个苯乙醇苷类、6个三萜类及16个其他类（糖类、黄酮类、核苷类等）成分。QAMS法和ESM法测得的各成分含量无显著性差异，5种成分相对误差（ RE）均低于5%。结论 通过UPLC-Q-TOF-MS/MS技术可实现对九味熄风颗粒化学成分的快速鉴定，建立的ESM与QAMS法联用的多指标定量方法可为该制剂酚类成分的质量一致性评价提供技术支撑。

Objective The chemical compositions of Jiuwei Xifeng Granules were analyzed by UPLC-Q-TOF-MS/MS technology, and a quantitative analysis of multi-components by single marker (QAMS) method was established for the determination of five phenolic acid components (gastrodin, parishin E, parishin B, parishin C, and parishin A). Methods The analysis was performed on a Waters UPLC HSS T₃ column (100 mm×2.1 mm, 1.8 μm) using a mobile phase of methanol-0.1% formic acid aqueous solution with gradient elution. The flow rate was 0.3 mL·min^-1, and the column temperature was maintained at 35 ℃. Electrospray ion source (ESI) was used to scan in positive and negative ion modes, and the components were identified according to the mass spectrometry data combined with literature reports. For quantification, a Phenomenex Luna C₁₈ column (250 mm×4.6 mm, 5 μm) was used with a mobile phase of acetonitrile-0.1% phosphoric acid aqueous solution (gradient elution) at a flow rate of 1.0 mL·min^-1 and a column temperature of 30 ℃. Detection was performed at 220 nm. Using gastrodin as the internal reference substance, relative correction factors were established for four phenolic compounds, and their contents were calculated. The differences between the external standard method (ESM) and QAMS were compared. Results A total of 92 chemical constituents were tentatively identified in Jiuwei Xifeng Granules, including 20 alkaloids, 20 organic acids and their esters, 12 iridoids, six phenols, six amino acids, six phenylethanoid glycosides, six triterpenoids, and 16 other components (such as sugars, flavonoids, nucleosides, etc.). The QAMS method and ESM showed no significant differences in the content determination of each component, with relative errors (RE) of all five components below 5%. Conclusion The UPLC-Q-TOF-MS/MS technique enables rapid identification of chemical components in Jiuwei Xifeng Granules, while the established multi-index quantitative method combining ESM and QAMS can provide technical support for the quality consistency evaluation of phenolic compounds in this preparation.

R283.6

江苏省基础研究计划自然科学基金-前沿引领技术基础研究专项（BK20232014）