UPLC-MS/MS法检测清热散结胶囊中阿多尼弗林碱

目的：建立清热散结胶囊中阿多尼弗林碱的含量检查方法。方法：采用UPLC-MS/MS法，以野百合碱为内标计算浓度。色谱分离采用ACQUITY UPLC BEH C₁₈色谱柱（2.1 mm×50 mm，1.7 μm），流动相为0.1%甲酸水溶液（A）-乙腈（B），梯度洗脱（0～2.5 min，6%B；2.5～4 min，6%B→40%B；4～9 min，40%B;9～11 min， 40%B→6%B；11～15 min，6%B），流速为0.3 mL· min^-1， 柱温为30℃，进样量2 μL;采用电喷雾离子源，多反应监测模式（MRM）检测。结果：阿多尼弗林碱浓度在0.001～ 0.046 μg·mL^-1范围内呈现良好线性关系（r=0.9990），加样回收率为95%～105%，RSD小于2.5%；方法重复性及精密度良好。结论：所建立的方法专属性强，灵敏度高，重复性好，适用于清热散结胶囊中阿多尼弗林碱的检测。

Objective: To establish a method for the detection of adonifoline in Qingre Sanjie capsules. Methods: UPLC-MS/MS method was used.Monocrotaline was used as an internal standard.Chromatography was performed on an ACQUITY UPLC BEH C₁₈ column(2.1 mm×50 mm,1.7 μm) at 30℃ using a gradient elution(0-2.5 min,6%B;2.5-4 min,6%B→40%B;4-9 min,40%B;9-11 min,40%B→6%B;11-15 min,6%B) of 0.1% formic acid in water(A)-acetonitrile(B) at the flow rate of 0.3 mL·min^-1.The injection volume was 2 μL.ESI source was used which was performed in the multiple reaction monitoring mode. Results: Good linearity was obtained for quantitation of adonifoline over the range of 0.001-0.046 μg·mL^-1(r=0.9990).And recoveries were between 95%-105% with RSD no more than 2.5%.Good reproducibility and precision were also achieved. Conclusion: The method is convenient,reliable and accurate,which is suitable for the detection of adonifoline in Qingre Sanjie capsules.

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