基于UHPLC-Q-TOF-MS的醋甘遂萜类化学成分研究

Analysis of Terpenoids in Kansui Stir-Baked with Vinegar by UPHLC-Q-TOF-MS

  • 摘要: 目的 应用UHPLC-Q-TOF-MS对醋甘遂的萜类化学成分进行定性分析。方法 采用ACQUITY UPLC C18 色谱柱(100 mm×2.1 mm,1.7 μm),以0.1%甲酸(A)-乙腈(B)溶液为流动相进行梯度洗脱,流速0.4 mL/min,柱温40 ℃,进样量4 μL。质谱为ESI离子源,正、负离子模式下进行检测。结果 通过Peak View SoftwareTM质谱分析软件,结合保留时间、质谱特征碎片和裂解途径等信息,并通过对照品及文献比对,从醋甘遂中推测鉴定出32个萜类化合物,包含15个巨大戟烷型二萜、12个假白榄烷型二萜以及5个三萜,并对其所含主要萜类化合物巨大戟烷型和假白榄烷型的裂解规律进行了归纳分析。结论 该方法可快速鉴别醋甘遂中的萜类化学成分,并根据质谱信息将其所含主要萜类化合物进行归类,从而为醋甘遂的毒-效物质基础和质量控制提供一定的参考。

     

    Abstract: OBJECTIVE To identify the terpenoids of Kansui stir-baked with vinegar by UHPLC-Q-TOF-MS/MS. METHODS Chromatographic separation was performed on an ACQUITY UPLC C18 column (100 mm×2.1 mm, 1.7 μm) with a gradient solvent system composed of 0.1% aqueous formic acid (A) and acetonitrile (B) at a flow rate of 0.4 mL/min, and the temperature of column was 40 ℃ with injection volume of 4 μL. The samples were analyzed with an electrospray ionization (ESI) interface set in both positive and negative ionization modes. RESULTS The terpenoids of Kansui stir-baked with vinegar were analyzed by Peak View SoftwareTM, 32 terpenoids were identified, including 15 ingenane diterpenes, 12 jatrophane diterpenes and 5 triterpenes. And the fragmentation of ingenane diterpenes and jatrophane diterpenes was analyzed. CONCLUSION This method is rapid and accurate, which can be applied for explaining the material basis and finding the possible mechanism of "toxicity-efficacy" of kansui stir-baked with vinegar.

     

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