UHPLC-ESI-MS/MS同时测定尿毒康合剂中11种成分的含量

    Simultaneous Determination of 11 Components in Niaodukang Mixture by UHPLC-ESI-MS/MS

    • 摘要:
      目的  建立UHPLC-ESI-MS/MS法同时测定尿毒康合剂中没食子酸、毛蕊异黄酮葡萄糖、芦丁、金丝桃苷、丹酚酸B、大黄酸、黄芪甲苷、隐丹参酮、大黄素、丹参酮I、丹参酮IIA的含量。
      方法 采用InertSustainR C18(3.0 mm×100 mm,3.0 µm)色谱柱,甲醇(A)-0.1%甲酸水溶液(B),梯度洗脱,流速0.4 mL·min−1,进样量20 μL;质谱采用电喷雾离子源(ESI 源),正负离子扫描切换,多重反应监测模式进行定量分析。
      结果 尿毒康合剂中11种成分在线性范围内峰面积与质量浓度均呈良好的线性关系,仪器精密度RSD<3.0%,加样回收率为98.44%~103.56%,RSD为2.04%~3.34%。
      结论 本方法高效、稳定、准确、简便,可用于尿毒康合剂中的质量评价与质量控制,并为尿毒康合剂中的临床应用及研究提供依据。

       

      Abstract:
      OBJECTIVE  To established a UHPLC-ESI-MS/MS method for simultaneous determination of gallic acid, calycosin-7-glucoside, rutin, hyperoside, salvianolic acid B, rhein, astragaloside IV, cryptotanshinone, emodin, tanshinone I, tanshinone IIA in Niaodukang mixture.
      METHODS InertSustainR C18(3.0 mm×100 mm, 3.0 µm) column was used, mobile phase was methanol(A)-0.1% formic acid(B) with gradient elution at a flow rate of 0.4 mL·min−1, and the injection volume was 20 μL.The mass spectrometry used the electrospray ionization source(ESI source). Multiple-reaction monitoring was employed with switching electrospray ion source polarity in positive and negative mode.
      RESULTS  The peak area and mass concentration of 11 components in Niaodukang mixture showed a good linear relationship within the linear range. The precision of RSD were <3.0%, the average recoveries ranged from 98.44% to 103.56%, RSD ranged from 2.04% to 3.34%.
      CONCLUSION The method is stable, accurate, and simple, which can be used to control and evaluate the quality of Niaodukang mixture. It can also provide evidence for clinical application and research of Niaodukang mixture.

       

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