双丹口服液的HPLC指纹图谱研究

HPLC fingerprint study of Shuangdan oral liquid

目的:建立双丹口服液冻干粉的高效液相色谱(HPLC)指纹图谱,为该药的质量控制提供依据。方法:色谱条件为:色谱柱ZORBAX SB C18(250mm×4.6mm 5μm,Agilent),柱温30°C,流动相为甲醇与2%冰醋酸。采用梯度洗脱程序:甲醇-2%冰醋酸(5∶95,v/v)0min,(5∶95)10min,(25∶75)30min,(40∶60)50min,(60∶40)70min,流速1mL/min,进样量20μL,检测波长280nm;以建立的HPLC分析方法对双丹冻干粉进行指纹图谱分析表征,确认各物质成分归属。结果:双丹冻干粉指纹图谱中有11个共有特征峰,其中1、6和11号峰分别为源自牡丹皮的没食子酸、芍药苷和丹皮酚,2、3、4、5、7、8、9和10号峰分别为源自丹参的丹参素、原儿茶酸、原儿茶醛、咖啡酸、紫草酸、迷迭香酸、丹酚酸B和丹酚酸A。结论:本次研究为后续双丹各制剂的整体质量描述和评价及双丹冻干粉给药后血中移行成分的分析奠定了基础,也为进一步探讨双丹方的物质基础及作用机制提供了依据。

Objective：To establish the HPLC fingerprints for the quality control of Shuangdan oral liquid and provide information on the therapeutic material bases of Shuangdan prescription.Methods：Separation was performed at 30℃ on ZORBAX SB C18（250mm×4.6mm 5μm,Agilent）with a mobile phase gradient（flow rate：1mL·min^1）prepared from methanol and 2% aqueous glacial acetic acid（v/v）.The detection wavelength was 280 nm.The method was applied for the identification of major components in chemical fingerprint of SD lyophilized powder.Results：11 main peaks exist in ten sample profiles were selected as the common peaks.The 11 compounds were simultaneously identified by UV spectrum and relative retention time compared with the reference standards.They are gallic acid,paeoniflorin and paeonol from Cortex Moutan and danshensu,protocatechuic acid,protocatechuic aldehyde,caffeic acid,lithospermic acid,rosmarinic acid,salvianolic acid B and salvianolic acid A from Radix Salvia Miltiorrhizae.Conclusion：This method could provide reference standard for the quality control of Shuangdan oral liquid and its related preparations,and could also provide more informations on the therapeutic material bases of Shuangdan prescription.