熟地黄饮片、标准汤剂、中间体、配方颗粒的相关性  

Correlation Analysis of HPLC Fingerprint of Pieces,Standard Decoction,Intermediates and Dispensing Granules of Rehmanniae Radix Praeparata

作　　者：李艳英 陈建红 李雪梅 LI Yan-ying;CHEN Jian-hong;LI Xue-mei(Peking University,Beijing 100871,China;Beijing Increase Pharm Co.Ltd.,Beijing 102200,China;Beijing Increase Innovative Drug Co.Ltd.,Beijing 102200,China)

机构地区：[1]北京大学,北京100871 [2]北京盈科瑞创新医药股份研究有限公司,北京102200 [3]北京盈科瑞创新药物研究有限公司,北京102200

出　　处：《中国实验方剂学杂志》2020年第3期146-155,共10页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：北京市“十病十药”科技攻关项目(Z161100001816023)。

摘　　要：目的:建立熟地黄饮片、标准汤剂、中间体、配方颗粒的HPLC指纹图谱,并对其质量相关性进行评价。同时结合出膏率和毛蕊花糖苷转移率等指标,评价熟地黄配方颗粒制备工艺的科学性和合理性。方法:采用HPLC法对多批次饮片、标准汤剂、中间体及配方颗粒进行指纹图谱检测和毛蕊花糖苷含量测定。指纹图谱方法采用Phenomenex Luna 100A C18(2)色谱柱(4.6 mm×250 mm,5μm),流动相乙腈-0.1%磷酸水,流速1.0 m L·min^-1,检测波长300 nm。毛蕊花糖苷含量测定方法参照2015年版《中国药典》熟地黄饮片项下方法。同时,结合出膏率和毛蕊花糖苷转移率,进行配方颗粒制备过程中量值传递相关性分析。结果:熟地黄饮片、标准汤剂、中间体中毛蕊花糖苷含量基本一致,熟地黄中间体、配方颗粒的出膏率、毛蕊花糖苷转移率均在标准汤剂标准范围之内且与标准汤剂基本一致;熟地黄17批饮片,17批标准汤剂,10批中间体及10批配方颗粒指纹图谱均呈现7个共有峰,呈良好的相关性;采用UPLC-Q-TOF-MS分析技术成分归属了熟地黄配方颗粒中13个主要色谱峰,对7个共有峰中4个共有峰进行了指认,分别为5-羟甲基糠醛、毛蕊花糖苷、异毛蕊花糖苷、地黄苷。结论:熟地黄饮片、标准汤剂、中间体、配方颗粒的主要化学成分组成基本相同,熟地黄配方颗粒制备工艺合理,建立的HPLC指纹图谱方法可用于熟地黄配方颗粒的生产全过程的质量控制。Objective:To establish HPLC fingerprint spectra of the pieces,standard decoction,intermediates,dispensing granules of Rehmanniae Radix Praeparata,and assess the quality correlation among them,then to evaluate the scientificity and rationality of preparation process based on the yields of dry extract and the transfer rate of acteoside.Method:Fingerprints of several batches of the pieces,standard decoction,intermediates and dispensing granules of Rehmanniae Radix Praeparata were detected by HPLC,and the content of acteoside was determined according to the method of ChP 2015.The fingerprint chromatographic separation was carried out on Phenomenex Luna 100 A C18(2)chromatographic column(4.6 mm×250 mm,5μm).The mobile phase was acetonitrile-0.1%phosphoric acid for gradient elution,with a flow rate of 1 mL·min^-1,and the detection wavelength was 330 nm.At the same time,the correlation analysis of quality transmission during the preparation of dispensing granules was carried out based on the yields of dry extract and the transfer rates of acteoside.Result:The contents of acteoside pieces,standard decoction and intermediates were basically consistent.The yield of dry extracts of intermediates and dispensing granules,and the transmission rate of acteoside were all within the range of standard decoction,and basically consistent with standard decoction.There were 7 common peaks in all fingerprint spectra of 17 batches of pieces,17 batches of standard decoction,10 intermediates and 10 dispensing granules of Rehmanniae Radix Praeparata,with a good correlation.The 13 main chromatographic peaks in the dispensing granules were identified by UPLC-Q-TOF-MS analysis,and 4 of the 7 fingerprint common peaks were identified as 5-hydroxymethyl furfural,acteoside,isoacteoside and martynoside.Conclusion:The main chemical constituents of Rehmanniae Radix Praeparata pieces,standard decoction,intermediates and dispensing granules are basically identical.The established HPLC fingerprint method can be used for the quality control of prepara

关 键 词：熟地黄 饮片 配方颗粒 标准汤剂 中间体 

分 类 号：R289[医药卫生—方剂学] R284.1[医药卫生—中药学]