基于HPLC-ELSD特征图谱及多元功效成分定量分析的炒酸枣仁配方颗粒质量标准研究

Quality Standard Study of Ziziphi Spinosae Semen Granules Based on the HPLC-ELSD Specific Chromatogram and Multiple Ingredients Determination

目的:建立炒酸枣仁配方颗粒HPLC-ELSD特征图谱及多元功效成分定量分析方法。方法:采用HPLCELSD法,以乙腈-0.1%甲酸溶液为流动相,梯度洗脱,建立炒酸枣仁配方颗粒特征图谱,并利用对照品和LC-MS法对其共有峰进行鉴定;同时建立腺苷、棘苷、6-阿魏酰斯皮诺素、酸枣仁皂苷A、酸枣仁皂苷B的含量测定方法。结果:建立了炒酸枣仁配方颗粒的HPLC-ELSD特征图谱,并以棘苷为参照峰,标定了17个共有峰,鉴定了其中10个峰;各样品图谱与对照图谱相似度均大于0.9。所测定的5个成分在测定浓度范围内均有良好的线性关系,平均加样回收率96.3%~98.1%,RSD均小于3.5%。结论:该方法简单快速、准确可靠、重现性好,可用于炒酸枣仁配方颗粒的质量控制。

Objective： To establish the specific chromatogram（ HPLC-ELSD） and multiple ingredients determination method of Ziziphi Spinosae Semen. Methods： HPLC-ELSD method was used to establish the specific chromatogram of Ziziphi Spinosae Semen granules,and acetonitrile-0. 1% formic acid solution was used as the mobile phase with the gradient elution. The common peaks were identified by comparison with the reference standards and LC-MS. At the same time,the method for simultaneous determination of adenosine,spinosin,6-feruloyl spinosin,jujuboside A and jujuboside B was established with the same approach. Results： HPLC-ELSD specific chromatogram of Ziziphi Spinosae Semen granules was established,and 17 peaks were defined as the common peaks with spinosin as the reference peak,ten peaks had been identified. The similarities of the sample＇s chromatograms compared with the reference chromatogram were higher than 0. 9. The five markers determined in this assay exhibited good linear relationship in the determination range,and their average recovery rates were 96. 3% ~ 98. 1% with the RSD all less than 3. 5%. Conclusion： The method provided in the study is simple,accurate and reliable,which can be used for the quality control of Ziziphi Spinosae Semen granules.