怀地黄中地黄苷A,地黄苷D及益母草苷含量快速分析方法的建立

目的:建立一种快速测定怀地黄中地黄苷A,地黄苷D,益母草苷含量的方法。方法:应用近红外光谱技术(near infrared reflectance spectroscopy,NIRS)测得85-5,北京1号,白状元,沁怀,白选,沁怀郑共6个品种108份怀地黄样品的近红外光谱图,结合高效液相法(high performance liquid chromatography,HPLC)同时测定的样品中地黄苷A,地黄苷D,益母草苷的含量,并利用TQ软件将光谱信息与测得含量相关联,采用偏最小二乘法(partial least squares,PLS)建立怀地黄中地黄苷A,地黄苷D,益母草苷的定量分析模型。结果:模型的内部交叉验证决定系数(R2)分别为0.924 67,0.934 96,0.951 54,校正均方差(root mean square error of calibration,RMSEC)分别为0.016 6,0.015 9,0.022 8,验证均方差(root mean square error of prediction,RMSEP)分别为0.017 00,0.007 86,0.012 50,交叉验证均方差(root mean square error of cross validation,RMSECV)分别为0.032 13,0.030 36,0.069 22,以及性能指数(performance index,PI)分别为92.5,82.7,83.1;配对样本t检验显示NIR模型预测值与HPLC测得参考值的P分别为0.422,0.549,0.131,均0.05,表明两组数据无显著性差异。结论:该方法准确、快速、绿色,可用于怀地黄中地黄苷A,地黄苷D,益母草苷的定量分析。

Establishment of Rapid Method for Analysis of Content of Rehmaionoside A, Rehmaionoside D and Leonuride in Rehmanniae Radix

Objective: To establish a rapid analysis method for determining the contents of rehmaionoside A, rehmaionoside D and leonuride in Rehmanniae Radix.Method: Near-infrared spectra of six varieties of Rehmanniae Radix (108 samples) were obtained by near infrared diffuse reflectance spectroscopy (NIRS) technique. By using high performance liquid chromatography (HPLC) method, the contents of rehmannioside A, rehmaionoside D and leonuride were detected and their values were correlated with the spectra information by using TQ Software. Then the quantitative models of rehmaionoside A, rehmaionoside D and leonuride in Rehmanniae Radix were built by partial least squares (PLS).Result: The correlation coefficients (R²) of the models was 0.924 67, 0.934 96 and 0.951 54; the root mean square error of calibration(RMSEC) was 0.016 6, 0.015 9 and 0.022 8; the root mean square error of prediction (RMSEP) was 0.017 00, 0.007 86 and 0.012 50; the root mean square error of cross validation (RMSECV) was 0.032 13, 0.030 36 and 0.069 22; and the performance index (PI) was 92.5, 82.7 and 83.1 respectively. Besides, paired sample t-test showed that the P value of NIR and HPLC was 0.422, 0.549 and 0.131, all higher than 0.05, indicating that there was no significant difference between the two methods.Conclusion: The NIR method is accurate, rapid, and green. It can be used for quantitative analysis of rehmaionoside A, rehmaionoside D and leonuride in Rehmanniae Radix.