五加生化胶囊UPLC-MS指纹图谱研究

目的: 建立五加生化胶囊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: 色谱柱:ACQUITY UPLC BEH (2.1mm×50 mm,1.7 μm);流动相:乙腈(A)-0.1%甲酸和10 mmol·L^-1醋酸铵(B)梯度洗脱;柱温:40℃;流速:0.4 mL ·min^-1;进样量:8 μL;电喷雾接口,正离子模式,毛细管电压3.50 kV,锥孔电压35.00 V,离子源温度120℃,脱溶剂温度380℃,脱溶剂气N₂:500 L·h^-1,锥孔气N₂:50 L ·h^-1。 结果: 11批五加生化胶囊UPLC-MS指纹图谱中共标定了37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,确定4号、8号、9号、10号和30号峰分别为紫丁香苷、阿魏酸、甘草苷、异嗪皮啶和藁本内酯。 结论: 所建立的五加生化胶囊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,可用于五加生化胶囊质量的控制。

Objective: To develop a ultra-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS) method for chemical fingerprint analysis of Wujia Shenghua capsules. Method: A UPLC-MS system, an ACQUITY Waters Ultra-Performance Liquid Chromatographic coupled with a Micromass Quattro Premier XE electrospray ionization (ESI) source mass spectrometer was used. An ACQUITY UPLC BEH (2.1mm×50 mm, 1.7 μm) column was operated under a gradient of 10 mmol·L^-1 ammonium acetate and 0.1% formic acid in water. The parameters of mass spectrometer were optimized. The spectra were recorded in the m/z range of 100-1 000. Result: Among 11 batches Wujia Shenghua Capsules, 37 common peaks were defined and identified by UPLC-MS. By comparing MS spectra data with the authentic standards and literature, the original of common peaks were determined and peak 4, 8, 9, 10 and 30 were identified as syringin, ferulaic acid, liquirtin,isofmxidin and ligustilide, respectively. Conclusion: The developed fingerprint assay is specific and can be readily utilized for comprehensive evaluation and quality control of Wujia Shenghua capsules.

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