Optimization Of Alcohol Precipitation Process For Extract Of Carthamus Tinctorius And Salvia Miltiorrhiza And Investigation On The Encapsulated Loss Phenomena

The alcohol precipitation process of extract of Carthamus tinctorius and Salvia miltiorrhiza, combined with the agglomeration and encapsulated loss phenomena were studied in this paper. The alcohol precipitation process for extract of Carthamus tinctorius and Salvia miltiorrhiza were optimized; the encapsulated loss of the active components in the alcohol precipitation process of Salvia miltiorrhiza extract was studied. The main researches were as follows:1. To investigate the optimal alcohol precipitation parameters for extract of Carthamus tinctorius. The effects of different factors on the transfer rate of hydroxysafflor yellow A (HSYA) was studied via single factor experiments, including the final alcohol concentration of the liquor, the speed of stirring, the density of the extract, the temperature and the pH of the liquor. Based on the results of single factor experiments, the final alcohol concentration of the liquor, the speed of stirring, the density of the extract and the pH of the liquor were studied by an orthogonal test and a multiple guidelines grading method, and the transfer rate of HSYA, the yield and the purity of extract in the supernatant were used as comprehensive evaluation index. The optimal alcohol precipitation process of Carthamus tinctorius extract was as follows:the final alcohol concentration of the liquor 50%, the speed of stirring 500 r/min, the density of the extract 1.15 g/mL and the pH of the liquor 5.00.2. An orthogonal test and a multi-index grading method were adopted in the alcohol precipitation process of Salvia miltiorrhiza extract for optimizing the alcohol precipitation condition. The precipitation, the retention rate and purity of danshensu, protocatechualdehyde, salvianolic acid B, and the purity of these active components in the supernatant were used as indices of appraisal. The best alcohol precipitation technolgy was to add 90% alcohol at a constant rate of 60.9 mL/min to Salvia miltiorrhiza extract of 1.20 g/mL density until the endpoint alcohol concentration of liquor was 80%, with fixed stirring speed of 450 r/min.3. The effects of different factors on form of precipitation and the encapsulated loss of the active components in the alcohol precipitation process of Salvia miltiorrhiza extract were studied by single factor experiments, including the density of the extract, the concentration of adding alcohol, the speed of stirring and the speed of adding alcohol. As is known to all, the encapsulated loss phenomena occurred when precipitate agglomerated to parcel the liquid. The factors mentioned above had different influence on the encapsulated loss, the higher the density of extract, and the higher concentration of alcohol, the more the encapsulated loss. Too fast or too slow stirring speed both lead to more encapsulated loss, while the speed of adding alcohol had insignificant influence on the encapsulated loss.4. The micro morphology of the particles in the alcohol precipitation process of Salvia miltiorrhiza extract was studied by in situ FBRM and PVM. The diversity of the appearance and the size change of the particle were investigated, compared with the encapsulated loss of the active components. Besides, the effects of crucial factors, including the density of the extract and the concentration of adding alcohol, on morphology and account of particles in the alcohol precipitation process of Salvia miltiorrhiza extract were monitored by FBRM and PVM. The results indicated that the encapsulated loss of the active components had a closed relation with the morphology of particles. The fine particles got together and formed agglomerate, leading to the encapsulated loss. Combination of FBRM and PVM is a feasible tool for monitoring particles behavior in alcohol precipitation processes, providing population statistics and images information on line, and revealing the process of particles formation and agglomeration. FBRM and PVM can determine agglomeration critical-time quickly and accurately, the time of which the encapsulated loss happens, also be used as preferential quality control methods to avoid or reduce the encapsulated loss phenomena on alcohol precipitation process of Salvia miltiorrhiza.