| Based on near infrared spectroscopy, this article did researches on quick analysis method of compound preparation and online monitoring of Paris Rhizome saponin separation. Then we tried to develop the separation methods of Paris Rhizome saponin reference substance.Using near infrared diffuse reflectance spectroscopy, the analytical methods of the fast and simultaneous determinations for asipilin, paracetamol and caffeine contained in the compound paracetamol have been built by the partial least squares method. For the three drug components asipilin, paracetamol and caffeine, the correlation coefficients 0.99945, 0.99033 and 0.99936 have been obtained, the root mean square errors (RMSE) of the calibration samples were 0.313, 0.520 and 0.0301, and the RMSE-s of the prediction samples were 1.07, 0.464 and 0.309, respectively.The on-line quality control for the resin adsorption, impurity elution, and un-adsorption of steroidal saponin in the extraction processes of AB-8 resin has been studied by the near infrared diffuse reflectance spectroscopy using chemical pattern recognition. The optimal and quality-controlled extraction method has been established. After this method was repeatedly tested online and verified by model, it could be used for craft research and online quality control of manufacture.Based on the near infrared diffuse reflectance spectroscopy, chemometrics methods and chromatographic separation technique, we studied on the high efficiency and low cost preparation method of Paris Rhizome saponin reference substance.Taking colloid Paris Rhizome as research object and using the spectrum discrimination variable of NIR as index of the online collections of effusion, we could monitor the separation process of Paris Rhizome saponins and its aglycons on AB-8 macroporous adsorption resin. Then the separation quality of active components in the traditional Chinese medicine would be controllable. Due to this method, we got a Paris Rhizome aglycon of 95.5% purity. In the same way, we researched the separation process of pennigenin and diosgenin AB-8 macroporous adsorption resin . Their purities were 75.2% and 94.3%. Their recovery rates were 46.2% and 50.9%. Under the same conditions, floured Paris Rhizome was used as research object, and the purity of separated pennigenin was 24.7% and its recovery rate was 63.0%. The purity of separated diosgenin was 97.6% and its recovery rate was 77.3%. Taking 120g floured Paris Rhizome for amplification experiments ,we got 2.267g diosgenin which was 1.89% of materials. Its purity was 95.4% and its recovery rate was 76.4%. Taking this diosgenin as the material of the semi-HPLC, we achieved the goals of high capacity and efficient separation. The samples were repeatedly separated in ODS-C18 and we got the pure components:2.190mg Paris Rhizome saponinâ… and Paris Rhizome saponinâ…¡. Compared with the standard curve of reference substance, the purities of the two separated components were 102.8% and 100.6%. These were compliant with the reference substances of the traditional Chinese medicine. The result proved that the connection of NIR spectrum and chromatographic column separation technology in preparation of reference substance would help us to got low-cost reference substances with high capacity and productive rate.
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