Résumé
To study and establish a monitoring method for macroporous resin column chromatography process of salvianolic acids by using near infrared spectroscopy (NIR) as a process analytical technology (PAT).The multivariate statistical process control (MSPC) model was developed based on 7 normal operation batches, and 2 test batches (including one normal operation batch and one abnormal operation batch) were used to verify the monitoring performance of this model. The results showed that MSPC model had a good monitoring ability for the column chromatography process. Meanwhile, NIR quantitative calibration model was established for three key quality indexes (rosmarinic acid, lithospermic acid and salvianolic acid B) by using partial least squares (PLS) algorithm. The verification results demonstrated that this model had satisfactory prediction performance. The combined application of the above two models could effectively achieve real-time monitoring for macroporous resin column chromatography process of salvianolic acids, and can be used to conduct on-line analysis of key quality indexes. This established process monitoring method could provide reference for the development of process analytical technology for traditional Chinese medicines manufacturing.
Résumé
A separation technology of catalpol from Rehmannia with macroporpus adsorbent resins was investigated. The content of catalpol in the extract was determined by high performance liquid chromatography (HPLC). Nine different kinds of macroporous adsorbent resins were studied on the static capacity of adsorption and desorption, and D101 resin was best for the separation of the extraction solution of Rehmannia. The results showed that D101 resin had the highest static adsorption capacity of 69.2mg/g dry resin and its isotherm curve can be well described by Langmuir and Freudlich equation. The 5% ethanol elution on removal of the solvent under reduced pressure provided a brown powder, which was subjected to an open column chromatography on silica gel eluted with a CHCl3–MeOH gradient. The fraction eluted with CHCl3-MeOH (8∶2) was identified as catalpol and the purity of the compound was more than 90% purity by HPLC analysis. The yield of this separation technology was 6%.