摘要
目的 建立益肾涤浊丸的指纹图谱,并对其淫羊藿苷、大黄素和丹参酮ⅡA的含量进行测定,为益肾涤浊丸的质量控制提供依据。方法 采用高效液相色谱(HPLC)法,固定相为WondaSil C_(18)-WR色谱柱(250 mm×4.6 mm,5μm),流动相为0.2%磷酸水溶液-甲醇,流速为1 mL/min,采用梯度洗脱,在268 nm波长下进行检测。基于《中药色谱指纹图谱相似度评价系统(2012版)》软件,对10批次益肾涤浊丸的HPLC指纹图谱进行相似度分析。通过对比对照品与样品中各色谱峰的保留时间,确定样品中主要特征峰的化学成分,并归属指纹图谱指标成分。对10批样品中淫羊藿苷、大黄素和丹参酮ⅡA进行含量测定。结果 采用HPLC法建立的10个批次益肾涤浊丸指纹图谱相似度在0.803~0.999之间,共标示出12个共有峰,鉴定出淫羊藿苷、大黄素、丹参酮ⅡA三个特征峰。淫羊藿苷、大黄素和丹参酮ⅡA分别在线性范围(μg/mL)1.75~28.00、1.00~16.00、1.20~19.20内表现良好线性关系(r≥0.999 6),平均加样回收率分别为100.09%、99.70%、101.91%,RSD分别为0.435%、0.295%、1.851%。结论 本研究建立的益肾涤浊丸HPLC指纹图谱稳定可靠,含量测定准确,方法更具优势,可作为益肾涤浊丸质量控制的参考标准,为其质量评价提供科学依据。
Objective To establish HPLC fingerprint of Yishen Dizhuo Pills(YDP),determine the contents of icariin,emodin and tanshinone IIA,it provided a basis for the quality control of YDP.Methods Used HPLC,the stationary phase was WondaSil C18-WR column(250 mm×4.6 mm,5μm),the mobile phase was methanol-0.2%phosphoric acid,the elution condition was a flow rate of 1 mL/min and a detection wavelength of 268 nm.The similarity degrees of the fingerprints of 10 batches of YDP was evaluated by using the"Similarity Evaluation System of Chromatographic Fingerprint Spectrum of Traditional Chinese Medicine(2012 Edition)",the chemical composition of the main characteristic peaks in YDP was determined by comparing the retention time of each chromatographic peak in the reference substance and the sample,the components of each flavor medicine were attributed.The contents of icariin,emodin and tanshinone IIA in 10 batches of samples were determined.Results The fingerprint similarity of the 10 batches of samples was between 0.803-0.999,and a total of 12 common peaks were calibrated,and three of the main characteristic peaks were successfully identified,which were icariin,emodin and tanshinone IIA,they had good relationship in the linear range were 1.75-28.00μg/mL,1.00-16.00μg/mL,1.20-9.20μg/mL(r≥0.9996).The mean recovery rates were 100.09%(icariin,RSD=0.435%)、99.70%(emodin,RSD=0.295%)、101.91%(tanshinone IIA,RSD=1.851%).Conclusion The established HPLC fingerprinting method established in this study is stable and reliable,and the existing content determination methods had more advantages.It can be used as a reference standard for the quality control of YDP,and provide a scientific basis for its quality evaluation.
作者
彭爱娜
安俏颜
田素英
戴易良
PENG Aina;AN Qiaoyan;TIAN Suying(Department of Pharmacy,Zhaoqing Hospital of Traditional Chinese Medicine,Zhaoqing 526020,China;不详)
出处
《中国处方药》
2025年第24期27-31,共5页
Journal of China Prescription Drug
基金
肇庆市科技创新指导项目(250107230093099)。
