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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 HPLC fingerprint of Shuangdan oral liquid freeze-dried powder to provide the basis for the quality control of this drug. Methods: The chromatographic conditions were as follows: column ZORBAX SB C18 (250 mm × 4.6 mm 5 μm, Agilent) with a column temperature of 30 ° C. The mobile phase consisted of methanol and 2% glacial acetic acid. A gradient elution program was used: methanol-2% glacial acetic acid (5:95, v / v) 0 min, (5:95) 10 min, (25:75) 30 min, (40:60) , The flow rate of 1mL / min, the injection volume of 20μL, detection wavelength 280nm; established HPLC analysis of the freeze-dried powder Shuangdan fingerprinting characterization to confirm the ownership of the material composition. Results: There were eleven common peaks in the fingerprint of freeze-dried powder of Shuangdan, in which the peaks of Nos. 1, 6 and 11 were respectively gallic acid, paeoniflorin and paeonol derived from Paeonia Suffruticus, 2,3,4,5, Peaks 7, 8, 9 and 10 were danshensu, protocatechuic acid, protocatechuic aldehyde, caffeic acid, lithospermic acid, rosmarinic acid, salvianolic acid B and salvianolic acid A derived from Salvia miltiorrhiza. Conclusion: This study laid the foundation for the overall quality description and evaluation of the double Dan preparations and the analysis of the blood migration components after administration of the double Dan freeze-dried powder, and also provided the basis for further exploring the material basis and mechanism of action The basis.