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目的:建立HPLC-MS-MS法测定牛黄降压丸中芍药苷的含量。方法:采用HPLC-MS-MS法对牛黄降压丸中芍药苷进行含量测定,选用Agilent 20RBA×SB-C18反相柱(2.1 mm×30 mm,3.5μm)为色谱柱,流动相为甲醇-5 mmol·L-1甲酸铵(75∶25),流速0.4 mL·min-1,柱温25℃。质谱条件:电喷雾离子源(ESI),检测方式为多离子反应监测(MRM),负离子模式,用于定量分析的离子为m/z 525~449。结果:芍药苷的线性范围为20~2 000 mg·L-1(r=1.000 0);样品平均加样回收率为99.56%,RSD 0.86%。结论:该方法操作简便,快速,准确度好,能有效控制牛黄降压丸的质量。
Objective: To establish a HPLC-MS-MS method for the determination of paeoniflorin in Niuhuang Jiangya Wan. Methods: The content of paeoniflorin in Niuhuang Jiangya Pill was determined by HPLC-MS-MS. The column was separated on an Agilent 20RBA × SB-C18 column (2.1 mm × 30 mm, 3.5 μm) with methanol- 5 mmol·L-1 ammonium formate (75:25), flow rate 0.4 mL · min-1, column temperature 25 ℃. MS conditions: electrospray ionization source (ESI), detection mode is multi-ion reaction monitoring (MRM), negative ion mode, the ion used for quantitative analysis is m / z 525-449. Results: The linear range of paeoniflorin was 20-2 000 mg · L-1 (r = 1.000 0). The average recovery of paeoniflorin was 99.56% and the RSD was 0.86%. Conclusion: The method is simple, rapid, accurate, and can effectively control the quality of Niuhuang Jiangya Pill.