金银花药材、标准汤剂、中间体、配方颗粒指纹图谱及过程质量评价研究

Fingerprint and Process Quality Assessment of Raw Herbs, Standard Decoction, Intermediates and Dispensing Granules of Lonicerae Japonicae Flos

关键词:  金银花  指纹图谱  含量测定  标准汤剂  配方颗粒

Key words:  Lonicerae Japonicae Flos  fingerprint  content determination  standard decoction  dispensing granules

摘要:

目的 建立金银花药材、标准汤剂、中间体、配方颗粒的HPLC指纹图谱及多指标含量测定,并对其相关性进行评价。方法 采用Agilent Eclipse XDB C₁₈色谱柱(250 mm×4.6 mm,5 μm),以乙腈-0.1%乙酸水溶液为流动相进行梯度洗脱,流速为1.0 mL·min"^-1,检测波长266 nm,进样体积10 μL。结果 建立了金银花药材-标准汤剂-中间体及配方颗粒的多成分HPLC特征图谱,10批金银花药材、标准汤剂、中间体及配方颗粒指纹图谱均呈现15个共有特征峰,呈良好的相关性,在15个共有峰中指认出隐绿原酸、绿原酸、新绿原酸、断马钱子酸、咖啡酸、马钱苷、断氧化马钱子苷、芦丁、金丝桃苷、木犀草苷、异绿原酸B、异绿原酸A、异绿原酸C 13个成分,并采用外标法对其含量进行测定。结论 金银花药材-标准汤剂-中间体及配方颗粒的HPLC特征图谱相关性良好,13个特征成分同时测定的方法准确可靠,所建立质量评价模式能够反映金银花4种形态多成分的整体面貌,为金银花配方颗粒质量控制提供数据支撑。

Abstract:

OBJECTIVE To establish the HPLC fingerprint and multi-index content determination methods of the raw herbs, standard decoction, intermediates and dispensing granules of Lonicerae Japonicae Flos, and evaluate the correlations among them. METHODS The Agilent Eclipse XDB C₁₈ column(250 mm×4.6 mm, 5 μm) was adopted with acetonitrile-0.1% acetic acid solution as the mobile phase for conducting the gradient elution. The detection wavelength was set at 266 nm with a flow rate of 1.0 mL·min^-1. The injection volume was 10 μL. RESULTS HPLC characteristic spectrum was established for multi-component of raw herbs, standard decoction, intermediates and dispensing granules of Lonicerae Japonicae Flos. There were 15 common characteristic peaks in all fingerprint spectrum of 10 batches of raw herbs, standard decoction, intermediates and dispensing granules of Lonicerae Japonicae Flos, presenting a good correlation, 13 chemical compounds were identified including crypto chlorogenic acid, chlorogenic acid, neochlorogenic acid, secologanic acid, caffeic acid, loganin, secoxyloganin, rutin, hyperoside, cynaroside, isochlorogenic acid B, isochlorogenic acid A and isochlorogenic acid C, and external standard method was used to determine its content.CONCLUSION Correlation is good between fingerprint of raw herbs, standard decoction, intermediates and dispensing granules of Lonicerae Japonicae Flos. The method of simultaneous determination of 13 characteristic components is accurately and reliably. The established quality evaluation model can reflect the overall appearance of four forms of Lonicerae Japonicae Flos, provide data support for quality control of dispensing granules of Lonicerae Japonicae Flos.