健脾益肺鼻炎方标准汤剂特征图谱的建立及4种指标成分的含量测定  

Establishment of characteristic chromatogram and content determination of 4 index components in Jianpi yifei biyan prescription standard decoction

作　　者：宛鑫 李得堂[2] 张丽娟[3] 易美容 祝赫 何嘉仑[2] 陈洁[2] 唐洪梅[2] 丘振文[2] WAN Xin;LI Detang;ZHANG Lijuan;YI Meirong;ZHU He;HE Jialun;CHEN Jie;TANG Hongmei;QIU Zhenwen(The First Clinical Medical College,Guangzhou University of Chinese Medicine,Guangzhou 510405,China;Dept.of Pharmacy,the First Affiliated Hospital of Guangzhou University of Chinese Medicine,Guangzhou 510405,China;Dept.of Otolaryngology,the First Affiliated Hospital of Guangzhou University of Chinese Medicine,Guangzhou 510405,China)

机构地区：[1]广州中医药大学第一临床医学院,广州510405 [2]广州中医药大学第一附属医院药学部,广州510405 [3]广州中医药大学第一附属医院耳鼻喉科,广州510405

出　　处：《中国药房》2022年第16期1980-1985,共6页China Pharmacy

基　　金：广州市科技计划项目(No.202201020457);广东省基础与应用基础研究基金项目(No.2019A1515011745);广州中医药大学第一附属医院青年科研基金项目(No.2019QN22)。

摘　　要：目的建立健脾益肺鼻炎方标准汤剂的高效液相色谱(HPLC)特征图谱,筛选质量控制的指标成分并测定其含量。方法采用HPLC法,结合《中药色谱指纹图谱相似度评价系统(2004版)》建立10批健脾益肺鼻炎方标准汤剂的特征图谱,并进行相似度评价,确定共有特征峰;以特征图谱共有峰峰面积为变量,采用SPSS 26.0软件和SIMCA 14.1软件进行聚类分析(CA)、主成分分析(PCA)和正交偏最小二乘法-判别分析(OPLS-DA),筛选变量重要性投影(VIP)值大于1.5的差异性成分;采用同一HPLC法测定健脾益肺鼻炎方标准汤剂中升麻素和差异性成分的含量。结果10批健脾益肺鼻炎方标准汤剂共标定出24个共有特征峰,相似度均大于0.960,通过比对指认出8个特征峰。CA和PCA结果显示,10批样品可聚为3类;OPLS-DA结果显示,VIP值大于1.5的成分共有3个,由大到小依次为升麻素苷(2号峰)、毛蕊异黄酮葡萄糖苷(4号峰)、5-O-甲基维斯阿米醇苷(6号峰)。升麻素苷、毛蕊异黄酮葡萄糖苷、升麻素和5-O-甲基维斯阿米醇苷4种成分的线性范围分别为0.0107~0.2130、0.0078~0.1560、0.0080~0.1600、0.0098~0.1950μg(r>0.999);精密度、重复性、稳定性(24 h)试验的RSD值均小于2%;平均加样回收率分别为105.98%(RSD=1.75%,n=6)、98.06%(RSD=3.87%,n=6)、96.38%(RSD=4.03%,n=6)、104.17%(RSD=1.27%,n=6)。10批样品中上述4种成分的含量分别为12.12~18.87、3.86~6.40、3.10~4.27、11.17~15.79μg/mL。结论建立的HPLC特征图谱方法稳定可行,可用于健脾益肺鼻炎方标准汤剂的质量控制;升麻素苷、毛蕊异黄酮葡萄糖苷、升麻素和5-O-甲基维斯阿米醇苷可作为该标准汤剂质量控制的指标成分。OBJECTIVE To establish HPLC characteristic chromatogram of Jianpi yifei biyan prescription standard decoction,to select the quality control index components and determine their contents.METHODS HPLC method combined with Similarity Evaluation System of TCM Chromatographic Fingerprint(2004 edition)were used to establish the characteristic chromatogram of 10 batches of Jianpi yifei biyan prescription standard decoction;the similarity evaluation and common peaks identification were also carried out.Using common peak area of characteristic chromatogram as variables,SPSS 26.0 software and SIMCA 14.1 software were used to perform cluster analysis(CA),principal component analysis(PCA)and orthogonal partial least squares-discriminant analysis(OPLS-DA);differential components with variable important in projection(VIP)value greater than 1.5 were screened;the contents of cimifugin and differential components were determined by the same method.RESULTS A total of 24 common characteristic peaks were identified,and the similarities of 10 batches of samples were higher than 0.960;eight characteristic peaks were identified by comparison with reference substance.CA and PCA results revealed that the samples were classified into 3 categories.OPLS-DA analysis showed that 3 components with VIP value greater than 1.5,which were prim-O-glucosylcimifugin(peak 2),calycosin 7-O-β-D-glucopyranoside(peak 4)and 5-O-methylvisammioside(peak 6)in descending order.The linear ranges of prim-Oglucosylcimifugin,calycosin 7-O-β-D-glucopyranoside,cimifugin and 5-O-methylvisammioside were 0.0107-0.2130,0.0078-0.1560,0.0080-0.1600,0.0098-0.1950μg(r>0.999),respectively.RSD values of precision,repeatability and stability tests(24 h)were all less than 2%.Average recoveries were 105.98%(RSD=1.75%,n=6),98.06%(RSD=3.87%,n=6),96.38%(RSD=4.03%,n=6)and 104.17%(RSD=1.27%,n=6).The contents of the above 4 components in 10 batches of samples were 12.12-18.87,3.86-6.40,3.10-4.27 and 11.17-15.79μg/mL,respectively.CONCLUSIONS The established HPLC characteristic chro

关 键 词：健脾益肺鼻炎方 标准汤剂 特征图谱 化学计量法 

分 类 号：R917[医药卫生—药物分析学] R283[医药卫生—药学]