摘要
目的:建立正心降脂片的HPLC指纹图谱,为该制剂的质量控制提供参考依据。方法:采用Kromasil C_(18)色谱柱(4.6 mm×150 mm,3.5μm)进行色谱分离,使用乙腈-0.1%甲酸流动相系统进行梯度洗脱,流速0.8 mL·min^(-1),柱温25℃,检测波长254 nm。采用国家药典委员会颁发的中药色谱指纹图谱相似度评价软件(2012版)分析评价所构建的10批正心降脂片指纹图谱相似度。采用Q-Exactive轨道阱高分辨质谱技术和对照品比对鉴定共有峰成分。结果:构建了正心降脂片的指纹图谱共有模式并确认了其中的32个共有指纹峰,去除芦丁积分前后计算得到的10批正心降脂片指纹图谱与对照指纹图谱的相似度分别大于0.99和0.95。采用高分辨质谱技术共鉴定了26个共有峰,其中13个共有峰采用对照品比对进一步确认为3’-羟基葛根素、葛根素、3’-甲氧基葛根素、大豆苷、芦丁、木犀草素-7-O-葡萄糖醛酸苷、橙皮苷、大豆苷元、丹酚酸A、槲皮素、异鼠李素、橙黄决明素、大黄素。通过与组方中各单味药以及阴性样品的比对,对共有峰进行峰归属,32个共有峰涵盖了组方中全部8味药材。结论:本文所建立的正心降脂片HPLC指纹图谱方法简便、可靠,专属性强,结合共有峰的高分辨质谱定性分析,为正心降脂片的质量评价及药效物质基础研究奠定了基础。
Objective:To establish the HPLC fingerprint of Zhengxin Jiangzhi tablets for its quality evaluation.Methods:The separation was performed on a Kromasil C_(18)column(4.6 mm×150 mm,3.5μm)with acetonitrile-0.1%formic acid solution as mobile phase.The flow rate was 0.8 mL·min^(-1).The detection wavelength was 254 nm and the column temperature was 25℃.The similarity evaluation of 10 batches of Zhengxin Jiangzhi tablets was conducted by“Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System(2012 edition)”.The common peaks were identified by Q-Exactive Orbitrap HRMS and the reference substance.Results:The fingerprint of Zhengxin Jiangzhi tablets was established and a total of 32 common peaks were marked.The similarities between the 10 batches of Zhengxin Jiangzhi tablets and the control fingerprint were greater than 0.99 after integrating all the 32 common peaks,while the similarities between the 10 batches of Zhengxin Jiangzhi tablets and the control fingerprints were greater than 0.95 after removing the rutin integral.A total of 26 common peaks were identified by Q-Exactive Orbitrap HRMS.By comparing with reference substance,13 of the identified peaks by HRMS were further confirmed as 3’-hydroxy puerarin,puerarin,3’-methoxy puerarin and daidzein,rutin,luteolin-7-O-glucuronide,hesperidin,daidzein,salvianolic acid A,quercetin,isorhamnetin,aurantio-obtusin,emodin.The adscription of the 32 common peaks was analyzed by comparing the Zhengxin Jiangzhi tablets sample with each single herb and negative sample,and the 32 common peaks covered all the 8 herbs in the prescription.Conclusion:The established method is simple,stable and specific,which will lay a foundation for the quality evaluation and substance basis study of Zhengxin Jiangzhi tablets.
作者
崔小敏
何芳
晋玥媞
任慧
胡静
曲彤
李宁
陈志永
CUI Xiao-min;HE Fang;JIN Yue-ti;REN Hui;HU Jing;QU Tong;LI Ning;CHEN Zhi-yong(Shaanxi Academy of Traditional Chinese Medicine,Xi’an 710061,China;Xi’an C.P.Pharmaceutical Co.,Ltd,Xi’an,710043,China;Xi’an Medical University,Xi’an 710021,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2022年第8期1440-1447,共8页
Chinese Journal of Pharmaceutical Analysis
基金
陕西省重点研发计划一般项目(2022SF-557)
陕西省中医药研究院陕西省中医医院“苗圃计划”一般项目(2021-17)。
