| Proprietary Chinese medicine oral solution?PCM-OS?is a kind of Chinese medicine preparations with the Chinese herbal medicine as the main material,which has the function of treatment and health care.In the production process,in order to ensure the quality of oral solution,it is need to measure the main active ingredients,but the existing measurement methods need much reagents and cumbersome operation,so it is not easy to achieve the rapid determination and analysis.Near-infrared spectroscopy,as a fast,simple,and no reagent analysis technology,has been applied in many fields.Taking a kind of Proprietary Chinese medicine oral solution product?The active ingredient is polysaccharide?as an example,a method of rapid analysis for PCM-OS polysaccharide was established which was based on near infrared spectroscopy combined with chemometrics.A total of 1533 PCM-OS samples were collected and their spectral values were measured using a XDS Rapid Content? near-infrared grating spectrometer?scanning scope: 400-2498 nm,wavelength interval: 2 nm?.In addition,the polysaccharide content was determined by potassium permanganate titration,which was used as the reference value for NIR modeling and validation.693 samples were randomly selected used for validation,the remaining 840 samples were used for modeling and were also further randomly divided into calibration?420?and predicted?420?for 30 times.Calibration and prediction models were established for all divisions.The model parameters were optimized depending on the mean prediction effects of all divisions.In order to eliminate the baseline drift and tilt,using the Savitzky-Golay?SG?correction method to establish the full spectrum partial least squares?full-PLS?model,the optimal SG modes?derivative order d = 1,polynomial p = 2,smoothing points m = 39?was selected based on the prediction effects.In addition,in order to avoid the saturated absorption caused by water molecules in near-infrared spectroscopy,the upper value of the absorbance was selected by the absorbance upper optimization?AUO-PLS?method,and the waveband combinations were determined to be 400-1880 & 2088-2346 nm.In order to further extract the information and improve the prediction performance of the model,based on the SG calibration spectra of the 400-1880 & 2088-2346 nm waveband,SG-AUO-MW-PLS,SG-AUO-EC-PLS and SG-AUO-RRPC-PLS models were established by using the wavelength screening method such as moving window?MW?,equidistant combination?EC?and repetition rate priority combination?RRPC?.The errors between the predicted value of NIR and the measured value of standard method?RMSEPV?were 28.18,27.40,27.19(mg·L-1),respectively;the predictive correlation coefficients were 0.864,0.875,0.887,respectively.The SG-AUO-RRPC-PLS method achieves the best predictive effect and uses the least number of wavelengths?N = 94?.The results show that the near infrared analysis technique can be applied to the rapid quantitative analysis of PCM-OS polysaccharide,which is of great significance for the quality control of proprietary Chinese medicines.The proposed optimization method that was integrated by PLS,SG calibration,saturated absorption rejection?AUO?and wavelength screening?MW,EC,RRPC?,can effectively improve the accuracy of spectral analysis,which provides valuable reference for the further application of near infrared technology. |
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