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在熊胆粉粗提物的乙酸乙酯洗涤工艺中,需要根据原料的性质对所用洗涤溶剂的倍数进行调整,才能提高产品的纯度和产率。该文采用近红外光谱反映熊胆粉粗提物原料的整体性质,对这一工艺进行了优化。按照不同的熊胆粉粗提物和乙酸乙酯用量设计试验,采集熊胆粉粗提物的近红外光谱,提取出光谱数据的前8个主成分,同乙酸乙酯用量一起作为输入变量,对熊胆粉提取物成品的纯度和收率进行回归。试验共计40组,其中30组校正集,用于建立模型;10组验证集,用于对所建模型进行评估。所建模型的校正、内部交叉验证和外部验证结果满意,纯度模型的相关系数分别为0.902,0.896,0.883,校正误差均方根(RMSEC),交互验证均方根误差(RMSECV),预测误差均方差(RMSEP)分别为1.22%,1.48%,1.59%。收率模型的相关系数分别为0.921,0.859,0.916;RMSEC,RMSECV,RMSEP分别为1.39%,1.65%,1.53%。结果表明,熊胆粉粗提物的近红外光谱结合乙酸乙酯用量可准确预测所得成品的纯度和收率,利用所建模型可以根据熊胆粉粗提物的性质优选出最为合适的乙酸乙酯用量,提高熊胆粉提取物的纯度和收率。
In the process of washing the crude extract of bear gall powder with ethyl acetate, the multiple of the washing solvent used needs to be adjusted according to the nature of the raw material to improve the purity and yield of the product. This article uses near-infrared spectroscopy to reflect the overall properties of raw material of bear gall powder crude extract, which has been optimized. According to the different amounts of crude extract of gall powder and the amount of ethyl acetate design experiment, the crude extract of the gall nut powder was collected by near infrared spectroscopy to extract the first eight main spectral components of the data, together with the amount of ethyl acetate as an input variable, Return the purity and yield of bear gall powder extract products. A total of 40 groups of experiments, of which 30 sets of calibration set for the establishment of models; 10 sets of validation set for the model to be assessed. The correlativity of the model, the internal cross-validation and the external validation were satisfactory. The correlation coefficients of the purity model were 0.902,0.896,0.883, RMSEC, RMSECV, and prediction error The variance (RMSEP) was 1.22%, 1.48%, 1.59% respectively. The correlation coefficients of the yield models were 0.921,0.859,0.916 respectively; RMSEC, RMSECV and RMSEP were 1.39%, 1.65% and 1.53% respectively. The results showed that the purity and yield of the obtained product can be accurately predicted by near infrared spectroscopy and the amount of ethyl acetate, and the most suitable acetic acid ethyl acetate can be selected according to the properties of crude extract of gall powder Ester dosage, improve the purity and yield of bear gall powder extract.