四消丸HPLC指纹图谱及化学模式识别研究

HPLC fingerprint and chemical pattern recognition of Sixiao Pills

目的:建立四消丸HPLC指纹图谱方法,为评价其质量提供参考。方法:采用Waters Symmetry Shield TM RP18色谱柱;乙腈(A)-0.1%磷酸溶液(B)为流动相,梯度洗脱;流速1.0mL·min-1;柱温30℃;检测波长254nm;进样量10μL。通过相似度评价、聚类分析、主成分分析和偏最小二乘判别分析对6家生产企业不同批次的四消丸样品进行质量评价和分析。结果:6家生产企业17批样品共标定24个共有峰,相似度为0.747~0.972,并对24个色谱峰进行了药味归属,同时指认了12个色谱峰;通过聚类分析及主成分分析将所有样品分为2类;偏最小二乘判别分析筛选出包括大黄素甲醚、大黄素葡萄糖苷、大黄素等在内的8种质量差异标志物。结论:该方法操作简便、准确,可用于四消丸的质量控制和评价研究。

OBJECTIVE To establish the HPLC fingerprint of Sixiao Pills to provide reference for the quality evaluation.METHODS The analyesis was carried out on Waters Symmetry Shield TM RP18 column,the mobile phase was acetonitrile(A)-0.1%phosphoric acid solution(B)by a gradient elution program,the flow rate was 1.0 mL·min-1,the column temperature was 30℃,and the sample injection volume was 10μL,the detection wavelength was 254 nm.The fingerprint similarity analysis,cluster analysis,principal component analysis(PCA)and orthogonal partial least squares discriminant analysis(PLS-DA)were performed to comprehensively evaluate the different batches of Sixiao Pills for 6 production enterprises.RESULTS A total of 17 batches of samples from six manufacturers with 24 common peaks were calibrated,The similarities of the tested samples were 0.747 to 0.972,and 24 chromatographic peaks were assigned to the source of medicinal materials,and 12 chromatographic peaks were identified;The cluster analysis and principal component analysis identification methods divide the samples into 2 categories;partial least square discriminant analysis screens out emodin methyl ether,emodin glucoside,emodin,etc.8 quality difference markers.CONCLUSION the method is simple,accurate,and it can be used to control and comprehensively evaluate the quality of Sixiao Pills.