摘要
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 develop quantitative analysis of multi-components with single marker（ QAMS） for determination of butylphthalide,senkyunolide A,and Z-ligustilide in Tianshu capsule. Method： An HPLC method was developed for simultaneous determination of butylphthalide,senkyunolide A and Z-ligustilide,and the chromatographic peaks were identified based on the UV spectra and accurate molecular weights obtained by UPLC-Q-TOF / MS. With butylphathlide as the internal substance, relative correction factors（ RCFs） of senkyunolide A and Z-ligustilide to butylphathlide were calculated at single wavelength and different wavelengths respectively through slope analysis method. Relative retention value method was used for positioning of chromatographic peaks; external standard method（ ESM） was used to verify the result accuracy. Result： QAMS method was established for the determination of butylphthalide,senkyunolide A and Z-ligustilide in Tianshu capsule and RCFs of senkyunolide A and Z-ligustilide to butylphathlide were 0. 272 and 1. 056,respectively. The contents of these three marker compounds were 0. 008%-0. 036%,0. 023%-0. 125% and 0. 028%-0. 084% in 18 batches of Tianshu capsule samples. No significant differences on the quantitative results were found between QAMS and ESM. Conclusion： The established QAMS method with butylphathlide as the internal substance could be used for the determination of butylphthalide,senkyunolide A and Z-ligustilide in finished products and manufacturing process of Tianshu capsule.
出处
《中国实验方剂学杂志》
CAS
CSCD
北大核心
2015年第22期86-93,共8页
Chinese Journal of Experimental Traditional Medical Formulae
基金
中国博士后基金项目(2012M510731)
中药制药过程新技术国家重点实验室开放基金项目(SKL2010M0204)
