基于UPLC指纹图谱及化学模式识别分析的四季三黄片质量一致性评价

Quality Consistency Evaluation of Siji Sanhuang Tablets Based on UPLC Fingerprint and Chemical Pattern Recognition

目的:建立四季三黄片超高效液相色谱法指纹图谱,并结合化学识别模式对其质量一致性进行评价。方法:ShimadzuShim-packgistC_(18)色谱柱(100 mm×2.1mm,2μm),以乙腈-0.1%三氟乙酸水溶液为流动相,梯度洗脱,体积流量为0.3 mL·min^(-1),柱温为30℃,检测波长为254 nm。采用相似度评价、聚类分析、主成分分析和偏最小二乘法-判别分析等模式识别技术对四季三黄片批次间质量差异进行分析。结果:指纹图谱有21个共有峰。4家生产企业的23批样品相似度为0.442~0.999,筛选出了影响质量的11个差异性标志物,结果表明不同企业样品质量存在较大差异,3家企业内批间一致性较好,1家企业内批间一致性较差。结论:建立的方法简便可行,具有良好的准确性、稳定性和专属性,能科学评价四季三黄片质量一致性,可为四季三黄片的质量控制提供参考。

Objective:To establish the ultra-performance liquid chromatography(UPLC)fingerprint of Siji Sanhuang Tablets,and evaluate its quality consistency by combining the chemical pattern recognition.Methods:Chromatographic separation was performed on a Shimadzu Shim-pack gist C_(18)(100 mm×2.1 mm,2µm)with a gradient elution of acetonitrile0.1%trifluoroacetic acid at the flow rate of 0.3 mL·min^(-1).The column temperature was 30℃,and the detection wavelength was 254 nm.The similarity evaluation,hierarchical cluster analysis(HCA),principal component analysis(PCA)and partial least squares discriminant analysis(PLS-DA)were conducted to evaluate the differences between batches of Siji Sanhuang Tablets.Results:The fingerprints were established with 21 common peaks.The similarity of 23 batches of samples from four manufacturers was 0.442-0.999,and eleven differential markers that caused quality differences were found.The analysis results showed that there were some differences among the samples from different manufacturers,and the inter-batch consistency of three manufacturers was good,except for one manufacture.Conclusion:The established method was simple,reproducible,stable and specific,and could evaluate the quality consistency of the samples comprehensively and systematically.This study provided reference for the overall quality evaluation of Siji Sanhuang Tablets.