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目的:建立天舒胶囊中丁基苯酞、洋川芎内酯A和Z-藁本内酯的一测多评法。方法:采用HPLC建立丁基苯酞、洋川芎内酯A和Z-藁本内酯的同步测定法,基于在线全波长扫描光谱和UPLC-Q-TOF/MS提供的精确相对分子质量确证待测色谱峰;以丁基苯酞为内参物,通过斜率法分别于单一波长和不同波长下计算丁基苯酞对洋川芎内酯A和Z-藁本内酯的相对校正因子,并用相对保留时间对待测色谱峰进行定位;采用外标法进行测定结果准确性验证。结果:建立了天舒胶囊中3种成分的一测多评质量评价模式,洋川芎内酯A和Z-藁本内酯对丁基苯酞的相对校正因子分别为0.272和1.056;18批次天舒胶囊样品中三者含量范围分别为0.008%~0.036%,0.023%~0.125%,0.028%~0.084%;外标法和QAMS测定结果无差异。结论:建立的以丁基苯酞为内参物,测定洋川芎内酯A和Z-藁本内酯含量的一测多评质量评价模式,适合用于天舒胶囊成品和生产过程的质量控制。
Objective: To establish a multi-evaluation method for determination of butylphthalide, yangchongxiong A and z-ligustilide in Tianshu capsule. Methods: Simultaneous determination of butylphthalide, yangchongxiong lactone A and Z-ligustilide by HPLC was confirmed based on the on-line full-wavelength scanning spectroscopy and the accurate relative molecular mass provided by UPLC-Q-TOF / MS Chromatographic peak; Butylphthalide as an internal reference material, by slope method at a single wavelength and at different wavelengths calculated Butylphthalide on the Chuanxiong lactone A and Z-ligustilide relative correction factor, and relative retention time The peak position of the measured chromatographic positioning; external standard method to verify the accuracy of the results. Results: The evaluation model of three ingredients in Tianshu capsule was established. The relative correction factors of yangchongxiong lactone A and Z-ligustilide to butylphthalide were 0.272 and 1.056, respectively. The 18 batches Tianshu capsule samples ranged from 0.008% to 0.036%, 0.023% to 0.125% and 0.028% to 0.084% respectively. There was no difference between the external standard method and the QAMS method. CONCLUSION: A multi-evaluation model for the determination of content of yangchuo xiong lactone A and z-ligustilide with butylphthalide as internal reference was established, which is suitable for the quality control of the finished product and production process of Tianshu capsule.