旋覆花-赭石药对酚酸类成分UPLC指纹图谱及多指标成分含量测定

Determination of Multiple Index Components and UPLC Fingerprint of Phenolic Acids in Inulae Flos-Haematitum Herb Pair

目的:建立旋覆花-赭石药对超高效液相色谱法(UPLC)指纹图谱及多指标成分含量同时测定的方法。方法:采用Agilent ZORBAX RRHD StableBond C_(18)色谱柱(100 mm×2.1 mm,1.8μm),以乙腈-0.1%磷酸水溶液为流动相梯度洗脱,流速为0.3 mL·min^(-1),检测波长为327 nm,柱温为35℃,进样量为1μL,建立旋覆花-赭石药对UPLC指纹图谱及同时测定新绿原酸、绿原酸、隐绿原酸、咖啡酸、异槲皮苷、异绿原酸B、1,5-二咖啡酰奎宁酸、异绿原酸C共8个指标成分含量的方法,并结合相似度评价、聚类分析(CA)及主成分分析(PCA)等化学模式识别方法对UPLC指纹图谱进行多元统计分析。结果:建立了旋覆花-赭石药对的UPLC指纹图谱,确定了16个共有峰,指认了其中8个成分。相似度评价结果表明,10批样品的相似度均大于0.990,CA及PCA均可将10批样品聚为3类。建立的含量测定方法稳定可靠,精密度、重复性、稳定性及加样回收率试验结果均良好。结论:建立的UPLC指纹图谱及同时测定8个指标成分含量的方法可用于旋覆花-赭石药对的质量控制。

Objective:To establish a method for simultaneously determining the UPLC fingerprint and the content of multiple index components in the Inulae Flos-Haematitum herb pair.Methods:The gradient elution was performed in Agilent ZORBAX RRHD StableBond C_(18) column(100 mm×2.1 mm,1.8μm)with the mobile phase composed of acetonitrile and 0.1%phosphoric acid aqueous solution at the flow rate of 0.3 mL·min^(-1),the detection wavelength of 327 nm,the column temperature of 35℃,and the injection volume of 1μL.The UPLC fingerprint of the herb pair was established.Meanwhile,the content of neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,caffeic acid,isoquercetin,isochlorogenic acid B,1,5-dicaffeoylquinic acid,and isochlorogenic acid C were determined.Further,similarity evaluation,cluster analysis,and principal component analysis were performed to analyze the UPLC fingerprint.Results:The UPLC fingerprint of the herb pair Inulae Flos-Haematitum was established,including 16 common peaks,among which 8 peaks were identified.The similarity of 10 batches of samples were greater than 0.990.The cluster analysis and principal component analysis divided the 10 batches of samples into three categories.The established content determination method was reliable,with good precision,repeatability,stability,and sample recovery.Conclusion:The established method for simultaneously determining the UPLC fingerprint and 8 index components can be used for the quality control of Inulae Flos-Haematitum herb pair.