| Objective: In this study, Angong Niuhuang Wan was selected as an example to develop rapid quality evaluation method. The key steps in the production process were confirmed. Based upon the characteristics of near infrared spectroscopy (NIR), the process analytical theories and methodologies of the application of NIR in Traditional Chinese Medicine (TCM) production were studied and then the quick quality evaluation methods of the raw materials, intermediates and products were established.Methods: The formula of Angong Niuhuang Wan is composed of Bezoar, Moschus, Cornu Bubali, Margaritifera, Cinnabaris, Realgar, Borneolum Syntheticum, Rhizoma Coptidis, Radix Scutellariae, Radix Curcumae and Fructus Gardeniae. The correlation analysis between the results of different measuring techniques was used to determine the marker and active ingredients. NIR spectra were used to evaluate the integrity and homogeneity.â… . The methods of rapid quality evaluation of the raw materials.â‘ The model of predicting the amount of artificial bezoar in the bezoar was constructed by NIR and support vector machine algorithm. Also the pretreatment methods of NIR spectra were given.â‘¡The content of geniposide in the Fructus Gardeniae and berberine in the Rhizoma Coptidis were determinered by HPLC. The wavenumber of NIR spectra best correlating to the content of geniposide and berberine were selected for regression analysis. The quality of Fructus Gardeniae and Rhizoma Coptidis were estimated by predicted geniposide and berberine content.â…¡. The methods of rapid quality assessment of the intermediates.â‘ S tudies on the correlation between NIR and the granularity of the Rhizoma Coptidis. The influence of the granularity to the mixture was studied by similarity calculation and samples with different granularity were discriminated by discrimination analysis.â‘¡The method of uniformity assessment of the intermediate. NIR spectra was used to judge the uniformity of the mixing process of the Angong Niuhuang Wan by similarity calculation. By this way the end point of the mixing process would be judged.â‘¢The method of rapid control of moisture content of Angong niuhuangwan Cufen. The predicting model of moisture content was set up by NIR with the wave band 10000-6000cm-1 and PLS algorithm.â‘£The method of rapid quality discrimination of the Angong Niuhuang Wan intermediates. To predict the integerity and homogeneity of the intermediates, typical samples of Angong Niuhuang Wan intermediate were confected. The similarity of the NIR spectra was calculated to evaluate the quality of the samples.â…¢. The predictmethod of rapid quality assessment of the Angong Niuhuang Wan. The principle marker components of Angong Niuhuang Wan were bilirubin, geniposide, baicalin and berberine. PLS algorithm was used to correlate the content determined by HPLC and NIR spectra. The predicting models of the content of bilirubin, geniposide, baicalin and berberine were constructed. The results of the similarity of NIR spectra can check out the Angong Niuhuang Wan rapidly .Results:â… .â‘ Different data processing methods have great influence to the results. The most suitable method was first derivative spectrum and fourth wavelet transform. The correlation coefficient and RESP of amount of artificial bezoar in the bezoar between NIR predicted and true were 0.9999 and 0.467% respectively.â‘¡The correlation coefficient of geniposide and berberine between the predicted value and determined value was 0.9902 and 0.9959 respectively. The RMSEC of predicting methods of geniposide and berberine was 0.437 and 0.086 respectively.â…¡.â‘ The repeatability of the Rhizoma Coptidis with small granularity(<0.154 mm) was better than that with larger granularity. Different granularity of samples can be discriminated by NIR.â‘¡The results showed that there was correlation between the NIR spectra and uniformity of the samples. The similarity was above 97% when the samples were mixed evenly, which matched the traditional method very well.â‘¢The correlation coefficient and RMSEC of the moisture of Angong niuhuangwan Cufen between the predicted and determined content were 0.9992 and 0.150 respectively.â‘£The similarity of the Angong Niuhuang Wan intermediates was above 98%, while that unqualified samples was less than 92%. The method could be used to discriminate and evaluate product rapidly. Besides, the qualified and unqualified products were at different district at the PCA chart.â…¢. The correlation coefficient of bilirubin, geniposide, baicalin and berberine of the Angong Niuhuang Wan between the predicted and determined content was 0.8187, 0.8402, 0.8243 and 0.8276 respectively. The RESP of bilirubin , geniposide , baicalin and berberine between the predicted and determined content was 7.25%, 4.68%, 1.55% and 2.32% respectively.Conclusion: In this study, the key steps and marker ingredients of Angong Niuhuan Wan manufacturing process were confirmed. The fast quantitative methods for the raw materials, intermediates and product were set up. The methods developed in this study can be used for granularity, uniformity and moisture control and provide references for the fast quality evaluation in the production process of other Chinese medicine pills.
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