吐根酊特征图谱研究与质量评价方法建立

目的: 建立吐根酊的HPLC特征图谱,对主要成分进行鉴别,并评价其质量。方法: 采用Inertsil ODS-SP(250 mm×4.6 mm,5 μm)色谱柱,以乙腈-0.4%甲酸水溶液为流动相,梯度洗脱,流速为1 mL·min^-1,检测波长210 nm,柱温35 ℃。利用LC-MS/MS方法对特征图谱中的主要特征峰进行推测,对其中的主要未知峰进行液相制备纯化,并用NMR试验进行结构鉴定。结果: 建立了40批吐根酊的HPLC特征图谱,推测其中的6个特征峰,对3个含量较大的色谱峰进行准确指认,分别为吐根酚碱、吐根碱和吐根苷。判断其中36批吐根酊样品为合格样品,4批为劣质吐根酊样品。结论: 建立的吐根酊HPLC特征图谱专属性强,方法验证表明其可用于该产品的质量评价。

Objective: To establish the HPLC specific chromatogram,identify the main constituents and evaluate the quality of ipecac tincture. Methods: The HPLC specific chromatogram was performed on an Inertsil ODS-SP column(250 mm×4.6 mm,5 μm)with a gradient mobile phase of acetonitrile -0.4% formic acid aqueous solution system at a flow rate of 1 mL·min^-1.The detection wavelength was 210 nm and the column temperature was 35 ℃.The main peaks in the chromatogram were presumed with LC-MS/MS.The main unknown peak was obtained by prepared HPLC and purified,and its structure was identified by NMR test. Results: The HPLC specific chromatograms of 40 batches of samples were obtained,in which six alkaloids were characterized and three main constituents were obtained and identified as cephaeline,emetine and ipecoside.Thirty-six samples were high qualified,while four samples were low qualified. Conclusion: The method validation shows that the established methods have high specificity and can be used for the quality evaluation of ipecac tincture.

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