ABSTRACT
OBJECTIVE：To establish the method for online rapid detection of related indexes in the concentration process of Huagai san extraction solution ，and to provide reference for judgment of concentration end point. METHODS ：Online diagram of 73 concentrated samples in the concentration process of Huagai san extraction solution were drawn by NIRS online collection equipment. The partial least squares （PLS）method was used to establish the NIRS quantitative calibration model of 5 related indexes （concentration density ， solid content ， the contents of amygdalin ， ephedrine hydrochloride and pseudoephedrine hydrochloride）. Another 15 samples were used to validate the model ，and the correlation of predicted value and measured value was analyzed. RESULTS ：The correlation coefficients （R2）of the concentration density ，solid content ，the contents of amygdalin ， ephedrine hydrochloride and pseudoephedrine hydrochloride in the quantitative calibration model were 0.982 5，0.999 9，0.998 3， 0.999 4 and 0.999 3，respectively；the root mean square errors of calibration （RMSEC）were 0.001 6，0.025 1，0.014 7，0.001 8 and 0.000 9；the root mean square errors of cross validation （RMSECV）were 0.002 1，0.035 8，0.033 6，0.006 3 and 0.001 3， respectively. After validation by 15 samples，root mean square errors of prediction （RMSEP）were 0.003 2，0.024 6，0.021 5， 0.007 7 and 0.005 9，respectively. CONCLUSIONS ：The established quantitative calibration model has good predictability and can provide basis for online judgment of concentration end point of Huagai san extraction solution.
ABSTRACT
Objective: To establish HPLC fingerprints of Huagai San and identificate the characteristic peaks ion and preparations- medicinal materials peak pattern matching. Methods: Similarity on 12 batches of Huagai San was estimated, and peak pattern matching of the original medicine was conducted. Sample extraction with methanol in ultrasonic condition was carried out. HPLC- DAD methods were developed, detection wave length was set at 280 nm, HPLC mobile phase consisted of acetonitrile-0.2% phosphate acid aqueous solution, volume flow-rate was delivered at 0.6 mL/min, and column temperature was kept at 30℃. Cluster analysis of 12 batches of Huagai San was analyzed by SPSS 19.0. Results: The results showed that 26 common peaks were defined, the peaks No. 4, 5, 10, 17, 18, 20, and 21 were ephedrine hydrochloride, pseudoephedrine hydrochloride, chlorogenic acid, liquiritin, glycyrrhizic acid, narirutin, and hesperidin, respectively, and peak pattern matching showed that Huagai San had 6, 3, 6, 1, 4, and 1 matching peaks with Ephedrae Herba, Mori Cortex, Citri Reticulatae Pericarpium, Armeniacae Semen Amarum, Glycyrrhizae Radix et Rhizoma, and Perillae Fructus, respectively. The fingerprint similarity among the samples was all over 0.960. All the samples were classified into three categories. Conclusion: Similarity evaluation combined with the peak matching of fingerprint for Huagai San could provide the scientific methods for its identification and quality control.