UPLC波长切换法同时测定脑安颗粒中9种化学成分的含量及其化学模式识别分析

Simultaneous Determination of Nine Components in Nao′an Granules by UPLC with Wavelength Switching and Combined with Chemical Pattern Recognition Analysis

目的:建立超高效液相色谱法(UPLC)波长切换法同时测定脑安颗粒中洋川芎内酯A、洋川芎内酯Ⅰ、洋川芎内酯H、川芎嗪、绿原酸、阿魏酸、阿魏酸松柏酯、羟基红花黄色素A和藁本内酯9种成分含量的方法。方法:采用Zorbax Eclipse Plus C18色谱柱(100 mm×2.1 mm,1.8μm),流动相为乙腈-0.4%冰醋酸溶液,梯度洗脱;流速为0.3 mL·min-1;检测波长为285、320、304 nm;柱温为30℃;进样量为2μL;并采用SPSS 22.0统计软件对含量测定结果进行主成分分析与聚类分析。结果:洋川芎内酯A、洋川芎内酯Ⅰ、洋川芎内酯H、川芎嗪、绿原酸、阿魏酸、阿魏酸松柏酯、羟基红花黄色素A和藁本内酯线性范围分别为5.17~82.68(r=0.9995)、5.01~80.08(r=0.9996)、4.84~77.48(r=0.9994)、2.03~32.62(r=0.9993)、3.47~55.56(r=0.9997)、3.16~50.62(r=0.9998)、3.63~58.04(r=0.9995)、3.12~49.88(r=0.9994)、8.56~136.96μg·mL^(-1)(r=0.9993);平均加样回收率为98.70%~100.01%,RSD均小于1.11%(n=6)。主成分分析与聚类分析均可将不同生产厂家的脑安颗粒很好地分类,且分类结果一致。结论:该方法简便、准确、重复性好,可用于脑安颗粒的质量控制。

Objective:To establish an Ultra performance liquid chromatography(UPLC)method for simultaneous determination of 9 components in Nao′an granules including senkyunolide A,senkyunolideⅠ,senkyunolide H,ligustrazine,chlorogenic acid,ferulic acid,coniferyl ferulate,hydroxysafflor yellow A,ligustilide.Methods:A Zorbax Eclipse Plus C18(100 mm×2.1 mm,1.8μm)chromatographic column was used;the mobile phase was acetonitrile(A)-0.4%glacial acetic acid solution(B)with gradient elution at the flow rate of 0.3 mL·min-1 and the detection wavelengths were 285,320 and 304 nm.The principal component analysis and cluster analysis were conducted for the results of content determination by SPSS 22.0 statistical software.Results:The linear ranges of senkyunolide A,senkyunolideⅠ,senkyunolide H,ligustrazine,chlorogenic acid,ferulic acid,coniferyl ferulate,hydroxysafflor yellow A,ligustilide were:5.17-82.68(r=0.9995)5.01-80.08(r=0.9996),4.84-77.48(r=0.9994),2.03-32.62(r=0.9993),3.47-55.56(r=0.9997),3.16-50.62(r=0.9998),3.63-58.04(r=0.9995),3.12-49.88(r=0.9994),8.56-136.96μg·mL^(-1)(r=0.9993),respectively.The average recoveries(n=6)varied from 98.70%to 100.01%with RSDs no more than 1.11%.The samples were clearly classification by using CA and PCA,and the results of classification were consistent.Conclusion:The method is simple and accurate with good repeatability,which can be used to control the quality of Nao′an Granules.