九味熄风颗粒HPLC指纹图谱及化学成分归属研究

HPLC Fingerprint Analysis and Chemical Compounds Identification of Jiuwei-Xifeng Granules

目的:构建九味熄风颗粒的HPLC指纹图谱,获得良好的各色谱分离峰形,获悉其成分归属与含量,准确客观评估九味熄风颗粒的整体质量。方法:采用高效液相色谱法,以Kromasil C18柱(250 mm×4.6 mm,5μm)为色谱柱,以乙腈-0.1%磷酸为流动相,梯度洗脱,检测波长225 nm,流速0.5 mL/min,柱温30℃。运用相关软件,以11批次的九味熄风颗粒为研究对象,计算其化学成分指纹图谱的相似度,指认图谱共有峰药材来源,结合飞行时间质谱法检测图谱中的主要化学成分。结果:建立了九味熄风颗粒的HPLC指纹图谱;发现并确定17个具有指纹意义的共有峰,可归属到6味药材,其中6个共有峰得到鉴定;各批次九味熄风颗粒样品指纹图谱与标准指纹图谱相似度均大于0.9。结论:该法准确快速获悉各批次原药材、中间体的成分变化,为合理调配提供试验数据支撑,最大程度保证成品的成分含量及组成比例的一致性。

Objective:To establish a method of fingerprint analysis on Jiuwei-Xifeng Granules by HPLC,and to obtain the good chromatographic separation peak patterns,to obtain the composition attribution and content,in order to evaluate the overall quality of Jiuwei-Xifeng Granules accurately and objectively.Methods:High performance liquid chromatography is used,the Kromasil C18(4.6 mm×250 mm,5μm)is used as the column,with acetonitrile-0.1%H3PO4 as the mobile phase for gradient elution.The detective wavelength is set at 225 nm,the flow rate is 0.5 mL/min and the column temperature is maintained at 30℃.Using relevant software,the chemical component fingerprint similarity of 11 batches of Jiuwei-Xifeng Granules is calculated,the source of the common peaks is identified and the main chemical components in the spectrum are detected by time-of-flight mass spectrometry.Results:HPLC fingerprints are developed for Jiuwei-Xifeng Granules;17 common peaks are determined,which are mainly attributed to 6 kinds of medicinal materials,and 6 of them are identified;the similarity is higher than 0.9 between the fingerprints of the different samples of Jiuwei-Xifeng Granules and the standard fingerprints.Conclusion:This method accurately and quickly obtains the changes in the composition of each batch of raw materials and intermediates,provides test data support for reasonable deployment,and ensures the consistency of the composition content and composition ratio of the finished product to the greatest extent.