摘要
目的建立银星养脑方超高效液相色谱(UPLC)指纹图谱,并测定指认出的4种成分的含量。方法色谱柱为ACQUITY UPLC?BEH C_(18)柱(100 mm×2.1 mm,1.7μm),流动相为0.1%磷酸水溶液-乙腈(梯度洗脱),流速为0.4 mL/min,检测波长为321 nm,柱温为30℃,进样量为1μL。采用中药色谱指纹图谱相似度评价系统(2012 A版)建立12批样品的UPLC指纹图谱,并进行相似度评价,确定共有峰并指认;采用聚类分析和主成分分析对样品进行分类和质量评价;采用UPLC法测定样品指认出的成分含量。结果12批样品UPLC指纹图谱中有30个共有峰,可确定归属银杏叶、蜜远志、川芎,指认出其中4种成分,分别为阿魏酸、3,6'-二芥子酰基蔗糖、异银杏素、金松双黄酮。样品相似度均大于0.990。样品共聚为4类;7个主成分累积方差贡献率达94.100%。4种成分质量浓度分别在3.36~67.20μg/mL,5.10~102.00μg/mL,5.00~100.00μg/mL,2.50~50.00μg/mL范围内与峰面积线性关系良好(R^(2)≥0.9980,n=5);精密度、稳定性、重复性试验结果的RSD均小于3.0%;平均加样回收率为99.01%~101.19%,RSD为0.22%~1.01%(n=6)。结论该方法简单可行、专属性强、重复性好,可用于银星养脑方的质量评价;也为银星养脑片的质量控制和二次开发奠定了前期基础。
Objective To establish the ultra-high performance liquid chromatography(UPLC)fingerprint of Yinxing Yangnao Formula and determine the contents of four identified components.Methods The chromatographic column was the ACQUITY UPLC®BEH C_(18) column(100 mm×2.1 mm,1.7μm),the mobile phase was 0.1%phosphoric acid aqueous solution-acetonitrile(gradient elution),the flow rate was 0.4 mL/min,the detection wavelength was 321 nm,the column temperature was 30℃,and the injection volume was 1μL.The UPLC fingerprint of 12 batches of samples was established and the similarity evaluation was performed by the Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine(Version 2012 A),the common peaks were marked and identified.The samples were classified and the quality was evaluated by the cluster analysis and principal component analysis.The contents of identified components in the samples were determined by the UPLC method.Results There were 30 common peaks in the UPLC fingerprint of 12 batches of samples,which from Ginkgo Folium,honey-baked Polygalae Radix and Chuanxiong Rhizoma;four components were identified,namely ferulic acid,3,6′-disinapoyl sucrose,isoginkgetin and sciadopitysin.The similarity of the samples was greater than 0.990.The samples were classified into four groups.The cumulative variance contribution rate of the seven principal components was 94.100%.The linear ranges of ferulic acid,3,6′-disinapoyl sucrose,isoginkgetin and sciadopitysin were 3.36-67.20μg/mL,5.10-102.00μg/mL,5.00-100.00μg/mL,2.50-50.00μg/mL(R^(2)≥0.9980,n=5)respectively.The RSDs of precision,stability and repeatability tests were all lower than 3.0%.The average recovery rate of the above four components was in the range of 99.01%-101.19%,with the RSDs in the range of 0.22%-1.01%(n=6).Conclusion This method is simple,feasible,specific and repeatable,which can be used for the quality evaluation of Yinxing Yangnao Formula,lay the foundation for the quality control and secondary development of Yinxing Yangnao Tablets.
作者
蒋翠平
陶叶琴
成紫嫣
严建业
熊丹
谢宗明
JIANG Cuiping;TAO Yeqin;CHENG Ziyan;YAN Jianye;XIONG Dan;XIE Zongming(Liuyang Hospital of Traditional Chinese Medicine,Liuyang,Hunan,China 410300;The Second Hospital of Integrated Traditional Chinese and Western Medicine Affiliated to Hunan University of Traditional Chinese Medicine,Liuyang,Hunan,China 410300;School of Pharmacy,Hunan University of Chinese Medicine,Changsha,Hunan,China 410208)
出处
《中国药业》
CAS
2024年第16期62-67,共6页
China Pharmaceuticals
基金
湖南省自然科学基金[2021JJ80070]
湖南省科技创新计划项目[2021SK51501]
湖南省长沙市自然科学基金[kq2202497]
湖南省长沙市中医药科研课题重点项目[A202304]。
