幼泻宁颗粒HPLC指纹图谱研究  

Study on HPLC fingerprint of Youxiening granules

作　　者：郑昆[1] 陈照宇 乔世琴 王金玉[1] 孙著叶 朱芹 ZHENG Kun;CHEN Zhao-yu;QIAO Shi-qin;WANG Jin-yu;SUN Zhu-ye;ZHU Qin(Rizhao Chinese Medicine Hospital,Rizhao 276800,China;Hunan Xiangtan Institute for Food and Drug Control,Xiangtan 411100,China)

机构地区：[1]日照市中医医院,日照276800 [2]湖南省湘潭市食品药品检验所,湘潭411100

出　　处：《药物分析杂志》2019年第10期1908-1914,共7页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立幼泻宁颗粒的HPLC指纹图谱,对市售幼泻宁颗粒的质量进行控制。方法:采用Agilent Zorbax-C18色谱柱(4.6 mm×250 mm,5μm),以乙腈(A)-0.3%磷酸水溶液(B)为流动相进行梯度洗脱,流速1.0 mL·min^-1,检测波长350 nm(0~40 min,检测木犀草苷及木犀草素)、220 nm(40~60 min,检测白术内酯Ⅰ、白术内酯Ⅱ和白术内酯Ⅲ),柱温30℃,进样量10μL。采用国家药典委员会《中药色谱指纹图谱相似度评价系统2004A版》对11批市售幼泻宁颗粒进行相似度评价,通过比对化学分离对照品的保留时间对主要特征峰进行明确化学指认并初步确定组方中药来源。结果:共确定幼泻宁颗粒HPLC指纹图谱21个共有峰,通过与对照品比较指认其中5个指标成分分别是木犀草苷(5号峰)、木犀草素(6号峰)、白术内酯Ⅰ(17号峰)、白术内酯Ⅱ(18号峰)和白术内酯Ⅲ(19峰),利用相似度软件对11批制剂指纹图谱进行分析,各批样品相似度均在0.95以上。建立的幼泻宁颗粒的HPLC指纹图谱的精密度、专属性、稳定性和重复性均良好。结论:该研究建立的幼泻宁颗粒HPLC指纹图谱基本能全面反映该中药复方制剂中各味组方的整体特征,可用于幼泻宁颗粒的质量控制和评价。Objective:To establish the HLC fingerprint of Youxiening granules,and to control the quality of commercial Youxiening granules. Methods:The separation was developed on an Agilent Zorbax-C18 column(250 mm×4.6 mm,5 μm)by gradient elution of acetonitrile(A)-0.3% phosphoric acid(B)at a flow rate of 1.0 mL·min^-1. The detection wavelength was 350 nm(0-40 min)for luteolin-7-glucoside and luteolin,and 220 nm(40-60 min)for atractylenolide Ⅰ,atractylenolide Ⅱ and atractylenolide Ⅲ. The column temperature was 30 ℃ and the sample volume was 10 μL. The similarities of 11 batches of commercially available Youxiening granules were evaluated by the National Pharmacopoeia Committee’s "Chinese medicine fingerprint similarity evaluation system 2004 A". The main characteristic peaks were identified by comparing with the retention time of the chemically separated reference substances and the origin of the prescription was preliminarily determined. Results:21 common peaks were selected in the fingerprint. By comparing with the mixed reference substances,5 indexes were identified as luteolin-7-glucoside(peak 5),luteolin(peak 6),atractylenolide Ⅰ(peak 17),atractylenolide Ⅱ(peak 18)and atractylenolide Ⅲ(peak 19). The similarities of all samples were above 0.95. The precision,specificity,stability and reproducibility of the method were satisfactory. Conclusion:The HPLC fingerprint of Youxiening granules established in this study can basically reflect the overall characteristics of each prescription in the compound preparation of Chinese medicine,and can be used for the quality control and evaluation of Youxie Ning granules.

关 键 词：幼泻宁颗粒 车前草 白术 炮姜 木犀草苷 木犀草素 白术内酯 指纹图谱 高效液相色谱 质量控制 

分 类 号：R917[医药卫生—药物分析学]