基于指纹图谱结合化学计量学的香砂平胃颗粒质量评价

Quality Evaluation of Xiangsha Pingwei Granules Based on Fingerprint Combined with Chemometrics

目的建立评价香砂平胃颗粒质量的高效液相色谱(HPLC)指纹图谱结合聚类分析(CA)及正交偏最小二乘判别分析(OPLS-DA)法。方法色谱柱为Waters XTERRA C_(18)柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.05%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为220 nm(苍术素、苍术醇)、284 nm(厚朴酚、和厚朴酚、橙皮苷、川陈皮素及甘草苷),柱温为25℃,进样量为10μL。以苍术素为参照,建立14批香砂平胃颗粒的HPLC指纹图谱;与对照品溶液比对,确定共有峰;结合化学计量学方法对制剂进行质量评价。结果确定23个共有峰,指认7个成分,分别为甘草苷、橙皮苷、苍术醇、苍术素、川陈皮素、和厚朴酚、厚朴酚;14批制剂的指纹图谱相似度为0.971~0.994;CA和OPLS-DA结果显示,14批样品聚为3类,表明不同年份样品间的质量存在一定差异;发现5个差异性标志物,分别为苍术醇、和厚朴酚、厚朴酚、7号峰和16号峰。结论所建立的HPLC指纹图谱结合CA及OPLS-DA方法,可有效评价香砂平胃颗粒的质量。

Objective To establish a high-performance liquid chromatography(HPLC)fingerprint combined with cluster analysis(CA)and orthogonal partial least squares-discriminant analysis(OPLS-DA)method for evaluating the quality of Xiangsha Pingwei Granules.Methods The chromatographic column was Waters XTERRA C_(18) column(250 mm×4.6 mm,5μm),the mobile phase was acetonitrile-0.05%phosphoric acid solution(gradient elution),the flow rate was 1.0 mL/min,the detection wavelengths were 220 nm(atractylodin and atractylol)and 284 nm(magnolol,honokiol,hesperidin,nobiletin and liquiritin),the column temperature was 25℃,and the injection volume was 10μL.The HPLC fingerprint of 14 batches of Xiangsha Pingwei Granules were established with atractylodin as the reference,the common peaks were determined by the comparison with the reference solution,and the quality of the preparation was evaluated by the HPLC fingerprint combined with chemometrics.Results Twenty-three common peaks were determined and seven components were identified,which were liquiritin,hesperidin,atractylol,atractylonin,nobiletin,honokiol and magnolol,respectively.The fingerprint similarity of 14 batches of preparations was in the range of 0.971-0.994.The results of CA and OPLS-DA showed that 14 batches of samples were grouped into three clusters,indicating that there were some differences in the quality of samples in different years.Five different markers were identified,which were atractylol,honokiol,magnolol,peak 7 and peak 16,respectively.Conclusion The established HPLC fingerprint combined with CA and OPLS-DA can effectively evaluate the quality of Xiangsha Pingwei Granules.