逍遥散UPLC-MS指纹图谱研究

目的: 建立逍遥散超高效液相色谱-质谱(UPLC-MS)的指纹图谱,为科学客观地评价其质量提供可靠的方法。 方法: 采用UPLC-MS法。色谱柱:Shim-pack XR-ODSⅡ(2.0 mm×75 mm);流动相:乙腈(A)-0.1%甲酸+10 mmol·L^-1甲酸铵(B);梯度洗脱5.0%(0 min),5.0%→50%(0~10 min),50%→80%(10~15 min),80%→95%(15~17 min);柱温:30℃;流量:0.3 mL·min^-1;进样量:8 μL。电喷雾接口,正离子模式;毛细管电压:3 kV;锥孔电压:35.00 V;离子源温度:110℃;脱溶剂温度:350℃;脱溶剂气:N₂:600 L·h^-1,锥孔气He:600 L·h^-1。 结果: 10批逍遥散UPLC-MS指纹图谱中共标定了16个共有色谱峰,通过与对照品的保留时间及质谱信息的比对,认定指纹图谱中的4号、6号和12号峰成分分别为阿魏酸、白术内酯Ⅲ和藁本内酯。 结论: 所建立的逍遥散UPLC-MS指纹图谱满足于方法学的要求,所得的指纹图谱特征性及专属性强,可用于逍遥散质量的控制。

Objective: To establish fingerprint by an ultra-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry(UPLC-ESI-MS),so as to provide a reliable method for scientific and objective evaluation of Xiaoyao San. Methods: An UPLC-MS system of an ACQUITY Waters UPLC coupled with a Micromass Quattro Premier XE ESI source mass spectrometer was used.An Shim-pack XR-ODS II column(2.0 mm×75 mm)was operated with a mobile phrase consisting of under a gradient elution of acetonitrile(A)-0.1% formic acid+10 mmol·L^-1 ammonium acetate(B)by gradient elution of 5.0%(0 min),5.0%→50%(0-10 min),50%→80%(10-15 min),and 80%→95%(15-17 min)at a column temperature of 30℃,the flow rate 0.3 mL·min^-1,the injection volume 8 μL.The analysis was performed with electric spr ay interface,under positive ion mode,the capillary voltage was 3 kV,the taper hole voltage 35.00 V,the ion source temperature 110℃,the temperature of the desolventizing agent 50℃,desolventizing gas N₂:600 L·h^-1,taper hole gas He:600 L·h^-1. Results: Among the 10 batches of Xiaoyao San,16 common peaks were defined and identified by UPLC-MS.By comparing MS data and retention time with those of the reference substances,peaks 4,6 and 12 were identified as peaks for ferulic acid,atractylenolide Ⅲ and ligustilide. Conclusion: The developed fingerprint assay is specific and highly featured which meets the methodological requirements and can be readily utilized for quality control of Xiaoyao San.

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