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目的采用近红外光谱技术建立快速测定防己药材有效成分含量及水分含量的方法。方法采用2015版《中国药典》防己项下相应方法测定防己药材中粉防己碱和防己诺林碱总量及水分含量,运用偏最小二乘法(PLS)建立其含量与NIR光谱之间的多元校正模型,采用相关系数(r)、校正均方根误差(RMSEC)、内部交叉验证均方根误差(RMSECV)和外部预测均方根误差(RMSEP)对校正模型进行优化和评价。利用校正模型对未知样品中粉防己碱和防己诺林碱总量及水分含量进行预测,检验模型的准确度。采用二阶导数法对光谱进行预处理,粉防己碱和防己诺林碱最佳建模波段在7891~3960 cm-1,水分最佳建模波段在8975~4032 cm-1。结果选择前8个主成分建立最优校正模型,粉防己碱和防己诺林碱总量的校正模型的r为0.9965,RMSEC为0.0347,RMSECV为0.136;而水分含量校正模型的r为0.9950,RMSEC为0.0458,RMSECV为0.263。经外部验证,粉防己碱和防己诺林碱校正模型的RMSEP和平均回收率分别为0.0964和100.8.%。而水分的分别为0.178和99.82%。结论所建方法具有简便快速、结果准确、无损样品的特点,可以应用于防己中粉防己碱和防己诺林碱总量及水分含量的快速测定。
Objective To establish a method for rapid determination of active ingredients and moisture content of antifungal herbs by near infrared spectroscopy. Methods The total amount and content of tetrandrine and nifedipine in Radix Angelicae Sinensis were determined by the corresponding methods of “Chinese Pharmacopoeia” in 2015, and the multivariate calibration between NIR spectra and content was established by partial least squares (PLS) Model, the calibration model was optimized and evaluated using correlation coefficient (r), root mean square error of correction (RMSEC), root mean square error of internal cross validation (RMSECV) and root mean square error of external prediction (RMSEP). The calibration model was used to predict the total amount and the content of tetrandrine and nimesin in the unknown samples to test the accuracy of the model. The second derivative method was used to pretreat the spectrum. The optimal modeling band for tetrandrine and forskolin was 7891-3960 cm-1, and the best modeling band for the water was 8975-4032 cm-1. Results The optimal calibration model was established by choosing the first eight principal components. The calibration model of tetrandrine and nimesulide was r = 0.9965, RMSEC = 0.0347, RMSECV = 0.136, and r = 0.9950 for RMSC, RMSEC 0.0458, RMSECV is 0.263. External validation showed that the RMSEP and the average recovery of tetrandrine and amphotericin calibration models were 0.0964 and 100.8%, respectively. While the moisture levels were 0.178 and 99.82% respectively. Conclusion The proposed method is simple, rapid, accurate and nondestructive. It can be applied to the rapid determination of the total amount of tetrandrine and anti-tubulin and the water content in Rhizoma.