青皮饮片、水煎液、配方颗粒的超高效液相色谱指纹图谱相关性研究

Correlationstudy on UPLC fingerprint of Citri Reticulatae Pericarpium Viride pieces,decoction and formula granules

目的建立青皮饮片、水煎液、配方颗粒超高效液相色谱(ultra performance liquid chromatography,UPLC)指纹图谱,并考察其相关性和差异性。方法采用UPLC法测定15批青皮饮片、水煎液、配方颗粒的指纹图谱,并对其进行相似度评价、斯皮尔曼(spearman)相关性分析、聚类分析(cluster analysis,CA)、主成分分析(principal component analysis,PCA)及正交偏最小二乘法判别分析(orthogonal partial least squares discriminant analysis,OPLS-DA)。结果青皮饮片、水煎液、配方颗粒的UPLC指纹图谱均确定了7个共有峰,并指认了辛弗林、芸香柚皮苷、橙皮苷、香蜂草苷、川陈皮素、橘皮素;15批青皮饮片、水煎液、配方颗粒指纹图谱与相应对照指纹图谱的相似度均大于0.890,三者对照指纹图谱的相似度均大于0.970;斯皮尔曼相关性分析结果显示,除橙皮苷外,青皮饮片、水煎液及其配方颗粒的其余6个共有峰均呈现显著的正相关性;CA、PCA及OPLS-DA结果均表明青皮水煎液与配方颗粒更为接近;OPLS-DA筛选出3个VIP值大于1的差异性标志物。结论青皮饮片、水煎液及配方颗粒的主要化学成分基本相同,并且具有较高的相关性,可为青皮配方颗粒的生产及质量控制提供参考。

Objective To establish the UPLC fingerprints of Citri Reticulatae Pericarpium Viride pieces,decoction and formula granules,and investigate their correlation and difference.Methods The fingerprints of Citri Reticulatae Pericarpium Viride pieces,decoction and formula granules were determined by UPLC method.The results were analyzed by similarity evaluation,spearman correlation analysis,cluster analysis(CA),principal component analysis(PCA)and orthogonal partial least squares discriminant analysis(OPLS-DA).Results The UPLC fingerprints of Citri Reticulatae Pericarpium Viride pieces,decoction and formula granules were identified 7 common peaks,and identified synephrine,narirutin,hesperidin,didymin,nobiletin and tangeretin.The similarity between the fingerprints of 15 batches of Citri Reticulatae Pericarpium Viride pieces,decoction and formula granules and the corresponding control fingerprints was more than 0.890,and the similarity of the three control fingerprints was more than 0.970.The result of Spearman correlation analysis showed that the common peaks,except hesperidin,of 15 batches of Citri Reticulatae Pericarpium Viride pieces,decoction and formula granules showed significant positive correlation.The result of CA,PCA and OPLS-DA showed that the decoction of Citri Reticulatae Pericarpium Viride was closer to the formula granules.OPLS-DA screened three differential components with VIP value more than 1.Conclusion The main chemical components of Citri Reticulatae Pericarpium Viride pieces,decoction and formula granules were basically the same,which can provide references for the production and the quality control of Citri Reticulatae Pericarpium Viride formula granules.