目的: 建立UPLC-MS/MS法测定千柏鼻炎片和千柏鼻炎胶囊中阿多尼弗林碱的含量,为市售制剂的质量控制提供参考。方法: 采用Waters ACQUITY UPLC BEHC18色谱柱(100 mm×2.1 mm,1.7 μm),以0.1%甲酸水溶液(A)-乙腈(B)为流动相,梯度洗脱,流速0.4 mL·min-1,柱温35 ℃。离子化模式为ESI+,多反应监测,m/z 366.15 →338.16(+)(定量离子),外标法测定。结果: 阿多尼弗林碱质量浓度在2.52~101.0 ng·mL-1范围内与峰面积呈现良好的线性关系(r=0.997 6),平均加样回收率为100.5%,检测限为1.01 ng·mL-1,定量限为2.52 ng·mL-1,精密度、重复性、稳定性考察符合分析要求。13家企业的137批次千柏鼻炎片和千柏鼻炎胶囊中阿多尼弗林碱含量在2.646 1~147.035 9 μg·g-1之间,不同生产企业以及个别生产企业的不同生产批次样品中阿多尼弗林碱含量差异较大。结论: 本研究所建立的方法简便、快捷、灵敏、准确,为含千里光药材制剂的肝毒性成分含量检测提供参考。
Objective: To establish an UPLC-MS/MS method for determination of adonifoline in Qianbai Biyan tablets and Qianbai Biyan capsules, in order to provide references for quality control of Qianbai Biyan tablets and Qianbai Biyan capsules. Methods: The assay was performed on the Waters ACQUITY UPLC BEHC18 column(100 mm×2.1 mm,1.7 μm) and the sample was eluted with a gradient mobile phase consisting of 0.1% formic acid (A) and acetonitrile (B), the flow rate was 0.4 mL·min-1, and the column temperature was 35 ℃.The MS system was operated by using electrospray ionization(ESI)in the positive ion mode, the scan mode was in multiple reaction monitoring(MRM)mode, m/z 366.15→338.16(+)(quantitative ion). External standard method was used in the experiment. Results: The calibration curves showed a good linear relationship in the ranges of 2.52-101.0 ng·mL-1 for the component (r=0.997 6), the average recovery rate was 100.5%, the low limit of detection was 1.01 ng·mL-1, and the low limit of quantification was 2.52 ng·mL-1, the RSDs of precision, repeatability and stability also met the analysis requirements. The content ranges of adonifoline in 137 batches of 13 drug companies were 2.646 1-147.035 9 μg·g-1. The content of adonifoline varies greatly among different drug companies and different batches of individual drug companies. Conclusion: The established method is simple, rapid, sensitive, accurate and can provide a reference for the content detection of hepatotoxic component in traditional Chinese medicine preparations containing Senecio scandens Buch.-Ham..
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