基于指纹图谱和4种指标成分的经典名方一贯煎基准样品量值传递分析

Quantitative value transfer analysis of benchmark sample of classical prescription Yiguan Decoction based on fingerprint chromatogram and four indicator components

目的建立经典名方一贯煎(Yiguan Decoction)基准样品HPLC指纹图谱,并对其指标性成分(5-羟甲基糠醛、阿魏酸、洋川芎内酯I、毛蕊花糖苷)进行含量测定,研究一贯煎基准样品量值传递规律,为复方制剂研制奠定基础。方法制备15批一贯煎基准样品,建立其HPLC指纹图谱,明确并归属特征峰;对一贯煎基准样品中指标性成分进行含量测定,分析指标性成分从饮片-基准样品的传递规律。结果15批一贯煎基准样品HPLC指纹图谱相似度>0.800,标定了29个共有峰,并对各共有峰进行药材归属,其中1号峰为北沙参、麦冬、当归、生地黄、枸杞子共有峰,2号峰为北沙参、麦冬、当归、生地黄、枸杞子、川楝子共有峰,3号峰为北沙参、当归、生地黄、枸杞子共有峰,4、13号峰为生地黄、枸杞子共有峰,5号峰为北沙参、枸杞子、川楝子共有峰,6号峰为生地黄、川楝子共有峰,7、8、10、17、24号峰为当归、枸杞子共有峰,11、20号峰为当归、生地黄共有峰,12号峰为当归、枸杞子、川楝子共有峰,15号峰为枸杞子、川楝子共有峰,18号峰为北沙参、枸杞子共有峰,19号峰为麦冬、当归、枸杞子、川楝子共有峰,29号峰为当归、生地黄、枸杞子、川楝子共有峰,14、22、25~28号峰为当归专属峰,23号峰为生地黄专属峰,9、16、21号峰为枸杞子专属峰。指标性成分5-羟甲基糠醛、洋川芎内酯I、阿魏酸、毛蕊花糖苷质量分数分别为90.3~144.1、75.6~166.2、105.4~200.3、149.9~293.3μg/g,转移率分别为15.53%~27.11%、38.36%~62.68%、16.23%~31.37%、31.41%~55.65%;测定15批一贯煎干膏率为42.95%~49.93%,传递率为84.39%~96.15%。结论采用指纹图谱、指标性成分含量测定及干膏率相结合的模式,对经典名方一贯煎基准样品的量值传递过程进行分析,可初步拟定一贯煎基准样品的质量标准,为其后续新药研发提供参考。

Objective To establish the HPLC fingerprints of the benchmark samples of Yiguan Decoction(YD,一贯煎),determine the contents of its index components(5-hydroxymethylfurfural,ferulic acid,senkyunolide I and verbascoside),and study the transfer pattern of YD benchmark samples,so as to lay the foundation for the development of compound formulations.Methods Fifteen batches of YD benchmark samples were prepared,then their HPLC fingerprints were established and their characteristic peaks were identified and assigned.The contents of the index components in the YD benchmark samples were determined,and the transfer pattern of the indicator components from the decoction pieces to the benchmark samples was analyzed.Results The similarity of the fingerprints of the 15 batches of YD benchmark samples was greater than 0.800,and 29 common peaks were calibrated and the medicinal materials of each common peak were assigned.Among these peaks,peak 1 was the common peak of Beishashen(Glehniae Radix,GR),Maidong(Ophiopogonis Radix,OR),Danggui(Angelicae Sinensis Radix,ASR),Dihuang(Rehmanniae Radix,RR)and Gouqizi(Lycii Fructus,LF);Peak 2 was the common peak of GR,OR,ASR,RR,LF and Chuanlianzi(Toosendan Fructus,TF);Peak 3 was the common peak of GR,ASR,RR and LF,peaks of 4 and 13 were the common peaks of RR and LF,peak 5 was the common peak of GR,LF and TF,peak 6 was the common peak of RR and TF,and peaks of 7,8,10,17 and 24 were common peaks of ASR and LF,peaks of 11 and 20 were common peaks of ASR and RR,peak 12 was common peak of ASR,LF and TF,peak 15 was common peak of LF and TF,peak 18 was common peak of GR and LF,peak 19 was common peak of OR,ASR,LF and TF,and peak 29 was common peak of ASR,RR,LF and TF,peaks of 14,22,25-28 were exclusive to ASR,peak 23 was exclusive to RR,and peaks of 9,16 and 21 were exclusive to LF.The mass fractions of 5-hydroxymethylfurfural,senkyunolide I,ferulic acid,and verbascoside ranged from 90.3 to 144.1μg/g,75.6 to 166.2μg/g,105.4 to 200.3μg/g,149.9 to 293.3μg/g,respectively.The transfer rates ranged from 15.53%to 27.11%,38.36%to 62.68%,16.23%to 31.37%,31.41%to 55.65%,respectively.The dry extract yield of the benchmark samples was in the range from 42.95%to 49.93%,and the transmission rate was in the range from 84.39%to 96.15%.Conclusion The combination of fingerprinting,dry extract yield and determination of the content of the indicator components was used to analyze the quantitative transfer process of the benchmark samples of the classical formula YD,which can initially formulate the quality standard of the benchmark samples of YD and provide reference for its future development of new drugs.