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研究黑顺片炮制过程中6种酯型生物碱的变化规律及特征图谱,为黑顺片的炮制原理研究奠定基础。采用Phenomenex Gemini C_(18)柱(4.6 mm×250 mm,5μm),流动相乙腈-40 mmol·L~(-1)醋酸铵(浓氨调pH 10.0)梯度洗脱,流速0.8 mL·min~(-1),检测波长235 nm,进样量10~20μL,测定6种酯型生物碱含量的变化以及建立炮制过程的特征图谱。随着炮制过程的进行,双酯型生物碱含量降低,单酯型生物碱变化规律不明显,各炮制过程环节的7种附子“状态”特征图谱差异明显。特征图谱中共标记13个峰,除6种已知单双酯型生物碱外,其余7个峰峰面积变化趋势与双酯型生物碱的变化趋势一致。该方法准确可靠,重复性好,可为揭示黑顺片炮制过程中指标成分的变化规律以及阐明炮制原理提供参考。
The study of the change rules and characteristic maps of six kinds of ester-type alkaloids in the process of Heshun tablets laid the foundation for the study of the processing principle of Heshun tablets. The mobile phase was eluted with a gradient of acetonitrile-40 mmol·L -1 ammonium acetate (conc. Ammonia adjusted to pH 10.0) on a Phenomenex Gemini C 18 column (4.6 mm × 250 mm, 5 μm) at a flow rate of 0.8 mL · min ~ (-1). The detection wavelength was set at 235 nm and the injection volume was 10 ~ 20 μL. The content of six kinds of ester alkaloids was determined and the characteristic map of the process was established. With the proceeding of processing, the content of diester alkaloids decreased and the variation regularity of monoester alkaloids was not obvious. There were significant differences among the seven kinds of aconites in the process of processing. 13 peaks were labeled in the characteristic map, except for the 6 known mono- and di-ester alkaloids, the trend of the other 7 peak areas was consistent with that of the diester alkaloids. The method is accurate and reliable and has good repeatability. It can provide a reference for revealing the changing law of index components during processing and the clarification principle.