近红外光谱法测定片仔癀中皂苷类成分的含量

Determination of saponins in Pien Tze Huang by near infrared spectroscopy

应用近红外光谱技术(near infrared spectroscopy,NIRS)对片仔癀锭剂及粉末中的皂苷类成分进行快速定量分析。采集片仔癀锭剂及其粉末的近红外光谱,采用高效液相色谱法(high performance liquid chromatography,HPLC)测定片仔癀中三七皂苷R1、人参皂苷Rg1和人参皂苷Rb1的含量作为参考值,通过OPUS处理软件将片仔癀的近红外光谱图与皂苷类成分含量的参考值进行关联,结合偏最小二乘法(partial least squares,PLS)分别建立各待测组分的定量分析模型,并对模型进行验证。结果显示,锭剂模型中三七皂苷R1、人参皂苷Rg1、人参皂苷Rb1及其总和的内部交叉验证均方差RMSECV(root mean square error of cross-validation)分别为0. 095 1,0. 555,0. 414,0. 960 mg·g-1,粉末模型的RMSECV分别为0. 085 6,0. 443,0. 405,0. 913mg·g-1,经外部验证,锭剂模型中三七皂苷R1、人参皂苷Rg1、人参皂苷Rb1及其总和的预测均方差RMSEP(root mean square error of prediction)分别为0. 111,0. 274,0. 276,0. 807 mg·g-1,粉末模型的RMSEP分别为0. 059 2,0. 322,0. 327,0. 705 mg·g-1,预测值与化学测定值的平均相对标准偏差均小于2. 0%,在α=0. 05水平进行配对t检验,预测集样品预测值与实测值间无显著性差异。该研究所建立的模型性能较好,对片仔癀中皂苷类成分含量预测准确,且该法操作简便、快速无损、环保,可用于片仔癀中皂苷类成分的快速检测和质量控制。

Near infrared spectroscopy(NIRS)was used for rapid quantitative analysis of saponins in Pien Tze Huang troches and powders.The near infrared spectra of Pien Tze Huang were collected,and the contents of notoginsenoside R1,ginsenoside Rg1 and ginsenoside Rb1 in Pien Tze Huang were determined by high performance liquid chromatography(HPLC)as the reference values.Then the near infrared spectra of the samples were associated with the reference values to establish the quantitative analysis models by using partial least squares(PLS)method.Finally,the models were verified by unknown samples.The results showed that root mean square error of cross-validation(RMSECV)of R1,Rg1,Rb1 and the total content was 0.095 1,0.555,0.414,0.960 mg·g-1 for the troches models,0.085 6,0.443,0.405,0.913 mg·g-1 for the powders models.After external validations,root mean square error of prediction(RMSEP)of R1,Rg1,Rb1 and the total content was 0.111,0.274,0.276,0.807 mg·g-1 for the troches models,0.059 2,0.322,0.327,0.705 mg·g-1 for the powders models.The averages of relative standard deviation between the predicted values and the chemical measured values were all less than 2.0%.According to the results of paired-t tests at the level ofα=0.05,there were no significant differences between the predicted values and the measured values.The established quantitative analysis models can be used to predict the contents of saponins in Pien Tze Huang accurately and the proposed method is simple,fast,non-destructive and environmentally friendly for the rapid detection and quality control of saponins in Pien Tze Huang.