目的 研究治疗帕金森病的中药复方芍地帕宁的化学组成及成分归属，以阐明其物质基础。方法 超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法(Ultra High Performance Liquid Chromatography/Quadrupole-Orbitrap Mass Spectrometer，UHPLC/Q-Orbitrap MS)，色谱柱 ACQUITY UPLC HSS T3 column(2。1 mm × 100 mm，1。8 μm，Waters)，流动相 0。1％甲酸水(A)和乙腈(B)，梯度洗脱(0～25 min，5％～18％B;25～30 min，18％～26％B;30～40 min，26％～57％B;40～45 min，57％～95％B;45～50 min，95％B)，流速 0。2 mL/min，柱温 30℃，进样量 2 μL;采用电喷雾离子源，分别于正、负离子模式下采集质谱数据;通过与对照品比对，以及色谱峰的MS、MS/MS谱图解析，对芍地帕宁方中化学成分进行结构鉴定。结果 共从芍地帕宁方中鉴别84个化合物，包括17个苯乙醇，10个单萜糖苷，13个游离酚，10个环烯醚萜，10个生物碱，7个硫酸酯，5个有机酸，4个酚类糖苷，4个氨基酸，4个核苷酸。通过与单味药进行比对，其中13个化合物来自熟地黄、11个来自白芍、16个来自鸡血藤、16个来自地龙、16个来自肉苁蓉、12个来自枸杞。结论 芍地帕宁方化学成分结构复杂多样，建立的UHPLC/Q-Orbitrap MS方法可系统、全面地阐明该方的化学组成，可为后续质量评价体系建立、活性药效成分筛选及作用机理阐释等研究奠定基础。
Chemical Analysis of Shaodi Paning Formula(芍地帕宁方)by UHPLC/Q-Orbitrap MS
Objective To study the chemical composition and component attribution of Shaodi Paning Formula(芍地帕宁方)for the treatment of Parkinson's disease in order to clarify its material basis.Methods The chemical constituents in Shaodi Paning Formula were qualitatively analyzed by using ultra-high performance liquid chromatography-quadrupole/orbitrap high resolu-tion mass spectrometry(UHPLC/Q-Orbitrap MS).The analyses were separated on an ACQUITY UPLC HSS T3 column(2.1 mm × 100 mm,1.8 μm,Waters)with 0.1％formic acid aqueous solution(A)-acetonitrile solution(B)as mobile phase using gradient elution system(0～25 min,5％～18％B;25～30 min,18％～26％B;30～40 min,26％～57％B;40～45 min,57％～95％B;45～50 min,95％B).The flow rate was set as 0.20 mL/min,the column temperature was set as 30℃,and the injection volume was 2 μL.Both of positive and negative modes MS and MS/MS data was acquired.The peaks in the formula were unambiguously identified by comparing with reference standards or tentatively characterized by analyzing their MS and MS/MS spectra.Results A total of 84 constituents were characterized,including 17 phenylethanoids,10 monoterpene glycosides,13 free phenolic compounds,10 iridoid,10 alkaloids,7 sulfates,5 organic acids,4 phenolic glycosides,4 amino acids and 4 nucleo-tides.Among these constituents,13 were from Shudihuang(Rehmanniae Radix Praeparata),11 from Baishao(Paeoniae Radix Al-ba),16 were from Jixueteng(Spatholobi Caulis),16 were from Dilong(Pheretima),16 were from Roucongrong(Cistanches Her-ba)and 12 from Gouqi(Lycii Fructus).Conclusion Structural diversity was observed in Shaodi Paning Formula.The chemical constituents in Shaodi Paning Formula could be comprehensively elucidated by using the established UHPLC/Q-Orbitrap MS method.This study also provided a foundation for the material basis for the following quality control,bioactive constituents screen-ing and action mechanism elucidation of Shaodi Paning Formula.
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