基于HPLC多成分定量控制联合化学计量学的妇科养荣胶囊质量评价研究

Study on quality evaluation of Fuke Yangrong Capsules based on HPLC multicomponent quantitative control combined with chemometrics

目的建立HPLC法同时测定妇科养荣胶囊中梓醇、地黄苷D、益母草苷、棕矢车菊素、异泽兰黄素、洋川芎内酯H、洋川芎内酯I、洋川芎内酯A和藁本内酯的含量的方法,结合化学计量学对其质量进行评价。方法采用Agilent Extend XDB-C18色谱柱(250 mm×4.6 mm,5μm);流动相乙腈-0.2%磷酸溶液,梯度洗脱,体积流量1.0 mL/min;柱温30℃,检测波长210 nm(检测梓醇、地黄苷D和益母草苷)、345 nm(检测棕矢车菊素和异泽兰黄素)和280 nm(检测洋川芎内酯H、洋川芎内酯I、洋川芎内酯A和藁本内酯);采用聚类分析、主成分分析等化学计量学方法对妇科养荣胶囊进行质量评价。结果 9种成分分别在5.53~110.60、1.97~39.40、2.29~45.80、0.66~13.20、1.74~34.80、1.36~27.20、2.68~53.60、3.41~68.20、 9.27~185.40μg/mL线性关系良好(r≥0.999 1),平均加样回收率(RSD)分别为99.91%(0.67%)、98.67%(1.18%)、 97.94%(1.07%)、 96.76%(0.96%)、 98.13%(1.32%)、 97.97%(1.66%)、 99.89%(0.87%)、100.11%(0.75%)、100.03%(0.84%);10批样品聚类分析分为2类,各成分含量差异与生产阶段有关。结论该方法操作简便、重复性好,可用于妇科养荣胶囊的质量控制。

Objective To set up an HPLC gradient elution method of catalpol, rehmannioside D, ajugol, jaceosidin, eupatilin,senkyunolide H, senkyunolide I, senkyunolide A and ligustilide in Fuke Yangrong Capsules simultaneously. Methods The Agilent Extend XDB-C18(250 mm × 4.6 mm, 5 μm) chromatographic column was used, with mobile phase composed of acetonitrile-0.2%phosphoric acid solution as a mobile phase in gradient elution, the flow rate was 1.0 mL/min, the column temperature was 30 ℃.The detection wavelength were 210 nm for catalpol, rehmannioside D and ajugol, 345 nm for jaceosidin and eupatilin, and 280 nm for senkyunolide H, senkyunolide I, senkyunolide A and ligustilide, Quality evaluation of Fuke Yangrong Capsules by cluster analysis and principal component analysis with SPSS 26.0 software. Results Nine constituents showed good linear relationships within the ranges of 5.53-110.60, 1.97-39.40, 2.29-45.80, 0.66-13.20, 1.74-34.80, 1.36-27.20, 2.68-53.60, 3.41-68.20,9.27-185.40 μg/mL(r ≥ 0.999 1), whose average recoveries were 99.91%, 98.67%, 97.94%, 96.76%, 98.13%, 97.97%, 99.89%,100.11% and 100.03% with the RSD of 0.67%, 1.18%, 1.07%, 0.96%, 1.32%, 1.66%, 0.87%, 0.75% and 0.84%, respectively. The samples of 10 batches of Fuke Yangrong Capsules could be divided into two categories, the content difference of each component is related to the production stage. Conclusion The simple,accurate and repeatable method can be used for quality control of multiple indicator components in Fuke Yangrong Capsules.