目的 建立UPLC-Q-TOF/MS^E結(jié)合UNIFI用于九味鎮(zhèn)心顆?；瘜W(xué)成分的快速檢測與鑒別方法。方法 采用UPLC-Q-TOF/MS^E技術(shù)對九味鎮(zhèn)心顆粒中的化合物進行分析，使用Waters Acquity UPLC BEH C₁₈色譜柱（100 mm×2.1 mm，1.7 μm），以0.1%甲酸水（A）-0.1%甲酸乙腈（B）洗脫（0~14 min，2% B；14.0~16.5 min，60% B；16.5~20.0 min，98% B），體積流量設(shè)為0.3 mL/min，柱溫為40℃，進樣量5 μL。質(zhì)譜分析采用電噴霧離子源，正、負離子模式下依賴MS^E方式采集數(shù)據(jù)，采集范圍為m/z 50~1 200，基于UNIFI在線軟件結(jié)合MassLynx軟件及人工審核進行化學(xué)成分鑒定與匹配。結(jié)果 實現(xiàn)了九味鎮(zhèn)心顆粒中89種化學(xué)成分的快速鑒別，其中有29個來源于君藥（人參、酸棗仁），47個來源于臣藥（茯苓、五味子、延胡索、遠志），12個來源于佐藥（地黃、天冬），1個來源于使藥（肉桂）。結(jié)論 建立的基于UPLC-Q-TOF/MS^E結(jié)合UNIFI方法首次對九味鎮(zhèn)心顆粒的化學(xué)成分進行快速的篩選，為發(fā)現(xiàn)中藥大復(fù)方中的非靶向分析和成分鑒定提供了新的視角，也可以為其物質(zhì)基礎(chǔ)、質(zhì)量控制的研究提供依據(jù)。

Objective To evaluate a method for rapid detection and identification of compounds in Traditional Chinese Medicine preparation based on UPLC-Q-TOF/MS^E and UNIFI software. Method UPLC-Q-TOF/MS^E was used to rapidly analyze chemical constituents of Jiuwei Zhenxin Granules, chromatographic separation was performed on an Waters Acquity UPLC BEH C₁₈(100 mm×2.1 mm, 1.7 μm) for gradient elution with the mobile phase of 0.1% formic acid solution (A) and 0.1% formate acetonitrile solution (B) for gradient elution (0-14 min, 2%B; 14.0-16.5 min, 60%B; 16.5-18.0 min, 98%B; 18-20 min, 98%B), the flow rate was 0.3 mL/min, the column temperature was 40℃, the injection volume was 5 μL. The mass spectrographic analysis was used with electrospray ionization (ESI), sample MS data was acquired by time-dependent MS^E in both positive and negative ion mode, the collection range was m/z 50-1 200. Chemical composition identification and matching based on UNIFI online software,Masslynx software and manual verification. Result Tatolly 89 chemical components in Jiuwei Zhenxin Granules was successfully identified, including 29 from principle drug (Ginseng and Semen Zizyphi spinosae), 47 from minister drug (Poria cocos, Chinese Magnoliavine fuit, Corydalis tuber, and Polygala tenuifolia), 12 from assistant drug (Rehmannia root and Asparagi radix), and 1 from envoy drug (Cinnamon). Conclusion The rapid method based on UPLC-Q-TOF/MS^E and UNIFI was achieved for screene of chemical components in Jiuwei Zhenxin granules for the first time. The study indicated that it is a practical method for non-targeted analysis and identification of compounds in Traditional Chinese Medicine preparation, and also give evidences for pharmacodynamic material and quality control of Traditional Chinese Medicine preparation.

R284.1

國家自然科學(xué)基金資助項目（81173541）