摘要
目的建立芪苓益肾颗粒物质基准的高效液相色谱指纹图谱,并建立同时测定其7种指标成分含量的方法。方法采用GL Sciences ODS-3(5μm,4.6 mm×250 mm)色谱柱,0.05%磷酸-水-乙腈为流动相梯度洗脱,流速1 mL·min^(-1),柱温35℃,检测波长254 nm。通过相似度分析,对共有峰进行归属。采用聚类分析,主成分分析及正交偏最小二乘法-判别分析对指纹图谱数据进行评价,并筛选关键性成分,测定7种活性成分的含量。结果15批芪苓益肾颗粒物质基准的对照指纹图谱的相似度均超过0.93,标定了22个共有峰,指认了18个色谱峰。15批物质基准分为两类,并筛选出5种关键性成分,分别是峰10(毛蕊异黄酮葡萄糖苷)、峰17(芒柄花苷)、峰18(毛蕊异黄酮)、峰1及峰20(芒柄花素)。同时测定了毛蕊异黄酮葡萄糖苷、阿魏酸、洋川芎内酯Ⅰ、芒柄花苷、毛蕊异黄酮、芒柄花素、藁本内酯共7种成分的含量,各物质基准的质量分数范围分别是1.09~1.68、0.27~0.63、0.06~0.45、0.51~0.99、0.31~0.68、0.29~0.59、0.25~0.96 mg·g^(-1)。结论该方法操作简单、重复性、稳定性较好,可为该制剂物质基准的质量控制与评价提供参考。
Objective To establish a high performance liquid chromatography (HPLC) fingerprint for the Qiling Yishen granules substance standard,and to simultaneously determine the contents of7 index components.Methods GL Sciences ODS-3 (5μm,250 mm×4.6 mm) chromatographic column was used with 0.05%phosphoric acid-water (A)-acetonitrile (B) as the mobile phase in gradient elution.The flow rate was 1 mL·min^(-1),the column temperature was 35℃,and the detection wavelength was 254 nm.The total peak was assigned by similarity analysis.Cluster analysis (CA),principal component analysis (PCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA) were used to evaluate the fingerprint data and screen the key components.The contents of 7 active ingredients was determined.Results The similarity of the control fingerprint spectrum based on the Qiling Yishen granule.Totally 22 consensus peaks were standardized,and 18columns peaks were identified.CA,PCA and OPLS-DA divided the 15 batches of material standards into two categories.Five key components were screened out,namely peak 10 (calycosin 7-O-β-D-glucopyranoside),peak 17 (formononetin),peak 18 (calycosin),peak 1 and peak 20 (formononetin).The contents of 7 components including verbasil glucoside,ferulic acid,ligustrideⅠ,formononetin,calycosin,formononetin,and ligustilide were at 1.09-1.68,0.27-0.63,0.06-0.45,0.51-0.99,0.31-0.68,0.29-0.59,0.25-0.96 mg·g^(-1).Conclusion The method is simple,reproducible,and stable,which can provide reference for the quality control and evaluation of the preparation material standard.
作者
王隆隆
杨忠杰
张海风
陈恒文
杜跃亮
吴作敏
王韵旨
宁萌
于晓涛
WANG Long-long;YANG Zhong-jie;ZHANG Hai-feng;CHENG Heng-wen;DU Yue-liang;WU Zuo-min;WANG Yun-zhi;NING Meng;YU Xiao-tao(Centralis Hospitalis Luohe,Luohe Henan 462300;Guang’anmen Hospital,China Academy of Chinese Medical Sciences,Beijing 100000)
出处
《中南药学》
CAS
2021年第12期2633-2639,共7页
Central South Pharmacy
基金
国家自然科学基金项目(No.82074396)
河南省医学科技攻关计划(No.LHGJ20191429)
漯医专[2021]207号(2021LYZKJXM046)
河南省工程研究中心(豫发改高技[2019]569号)
漯河市工程技术研究中心(漯科[2018]88号)
漯河市创新型科技团队(漯科[2018]88号)。
关键词
芪苓益肾颗粒
物质基准
指纹图谱
含量测定
Qiling Yishen granule
material standard
fingerprint
content determination