目的 采用UPLC-Q-TOF-MS/MS技術(shù)解析九味熄風(fēng)顆?；瘜W(xué)成分并建立5種酚酸類成分（天麻素、巴利森苷E、巴利森苷B、巴利森苷C、巴利森苷A）一測多評（ QAMS）定量測定方法。方法 應(yīng)用Waters UPLC HSS T₃色譜柱，以甲醇-0.1%甲酸水為流動相洗脫梯度，體積流量0.3 mL·min^-1，柱溫35℃，采用電噴霧離子源（ ESI），正、負(fù)離子模式掃描，根據(jù)質(zhì)譜數(shù)據(jù)結(jié)合文獻(xiàn)報道進(jìn)行成分鑒定。采用Phenomenex Luna C₁₈色譜柱，乙腈-0.1%磷酸水為流動相梯度洗脫，體積流量1.0 mL·min^-1，柱溫30℃，檢測波長220 nm，以天麻素為內(nèi)參物，建立其與4種酚類成分的相對校正因子，計算各待測組分的含量，比較外標(biāo)法（ ESM）和QAMS這2種方法的差異。結(jié)果 從九味熄風(fēng)顆粒中共推斷和鑒定出92個化學(xué)成分，包括20個生物堿類、20個有機(jī)酸及其酯類、12個環(huán)烯醚萜類、6個酚類、6個氨基酸類、6個苯乙醇苷類、6個三萜類及16個其他類（糖類、黃酮類、核苷類等）成分。QAMS法和ESM法測得的各成分含量無顯著性差異，5種成分相對誤差（ RE）均低于5%。結(jié)論 通過UPLC-Q-TOF-MS/MS技術(shù)可實現(xiàn)對九味熄風(fēng)顆?；瘜W(xué)成分的快速鑒定，建立的ESM與QAMS法聯(lián)用的多指標(biāo)定量方法可為該制劑酚類成分的質(zhì)量一致性評價提供技術(shù)支撐。

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

江蘇省基礎(chǔ)研究計劃自然科學(xué)基金-前沿引領(lǐng)技術(shù)基礎(chǔ)研究專項（BK20232014）