Studies On Process Analysis Of Silica-gel Column Chromatography Using Near Infrared Spectroscopy

The progress of TCM (Traditional Chinese Medicine) is blocked by the lack of fast and effective quality analytical techniques in manufacturing process. Researches on key manufacturing processes of TCM can help to solve the problem mentioned above, improve the industry's quality control level and promote the modernization of TCM. As a fast, nondestructive analytical method, NIRS (Near Infrared Spectroscopy) have been gradually applied in manufacturing process analysis of TCM in the past few years, and provided a possible solution for the problem. However, the researches and applications of the technology were not in-depth. In this thesis, analysis of silica-gel column chromatography process in TCM was studied, expecting to establish a fast quality analytical method using NIRS.This thesis aimed at the problem of the timing for collection of active ingredients in silica-gel column chromatography process.. Radix Paeonia Alba extract was studied as an example for establishment of a fast qualitative analysis method using NIRS. TLC (Thin layer chromatography) was used as a reference method, determining whether the elutes contained paeoniflorin or albiflorin. MD (Mahalanobis Distance) method was used to classify near infrared spectrum collected from column chromatography process. The accuracy of the established model was 96.4 %. This method was expected to supervise industrial manufacturing process.This thesis also established a fast analytical method for determination of the concentration of solanesol in Tobacco leave extract in silica-gel column chromatography process using NIRS. DPLS (Partial Least Squares Discriminant) was utilized to determine the time when solanesol was eluted, then PLSR (Partial Least Squares Regression) was utilized to construct the quantitive calibration model, which was applied to describe the elution curve of solanesol in Silica-gel column chromatography process. The results showed high accuracy close to the value measured by HPLC (High Performance Liquid Chromatography) .On-line NIRS was used for monitoring and measurement of the concentration of solanesol for Tobacco leave extract's silica-gel column chromatography process in this thesis. The proposed on-line method was nondestructive and accurate, could analyze silica-gel column chromatography directly and fast. The results were close to HPLC determined value, and competent to bedeveloped as an on-line monitoring and feedback-control method for TCM extracts' silica-gel column chromatography.