Preparation method for extracting and purifying tanshinone monomeric compounds from red sage root
A technology for tanshinone and compound, which is applied in the field of traditional Chinese medicine phytochemistry, can solve the problems of many operation processes, low proportion of tanshinone monomer compounds and high production cost, and achieves the effects of simple process, improved extraction rate and low cost
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Embodiment 1
[0023] Grind the salvia miltiorrhiza into 40-50 mesh salvia miltiorrhiza powder, weigh 120 grams of salvia miltiorrhiza powder, put it into a multi-stage countercurrent extraction device, add 1200 ml of 80% ethanol-phosphoric acid aqueous solution for countercurrent extraction for 5 hours, and filter after extraction , concentrated under vacuum (0.05-0.1MPa), and concentrated under reduced pressure at about 50°C to obtain 6.8 grams of crude tanshinone.
[0024] Take a glass chromatographic column with a column length of 450 mm and an inner diameter of 45 mm, and install 350 ml of D101 macroporous adsorption resin, load the crude tanshinone above on the top of the chromatographic column, and then use mobile phases of 50%, 60%, and 70%, 80%, 90% ethanol-water solution for gradient elution, followed by TLC plate, concentrated under vacuum (0.05-0.1MPa), and added water with absolute ethanol to obtain 0.19 g of Tanshinone I (purity 95.5%) , 0.42 grams of tanshinone IIA (purity 97....
Embodiment 2
[0033] Pulverize the salvia miltiorrhiza medicinal material into 40-50 mesh salvia miltiorrhiza powder, weigh 120 grams of salvia miltiorrhiza powder, put it into a multistage countercurrent extraction device, add 1200 ml of 80% methanol-glycine aqueous solution, and carry out multistage countercurrent extraction for 4 hours. The extract was filtered, and the filtrate was concentrated under vacuum (0.05-0.1 MPa), and concentrated under reduced pressure at about 55°C to obtain 6.5 grams of crude tanshinone.
[0034] Take a glass chromatographic column with a column length of 450 mm and an inner diameter of 45 mm, and install 250 ml of DM301 macroporous adsorption resin, load the above-mentioned crude tanshinone sample on the top of the column, and then use 50% and 60% mobile phase respectively. , 70%, 80%, 90% ethanol-water solution for gradient elution, TLC plate tracking, concentration under vacuum (0.05-0.1MPa), and water with absolute ethanol to obtain 0.18 grams of tanshino...
Embodiment 3
[0036] Pulverize the salvia miltiorrhiza medicinal material into 40-50 mesh salvia miltiorrhiza powder, weigh 120 grams of salvia miltiorrhiza powder, put it into a multistage countercurrent extraction device, add 1200 ml of 80% isopropanol-alanine aqueous solution, and carry out multistage countercurrent extraction at room temperature After extraction for 6 hours, the extract was taken out and filtered, and the filtrate was concentrated under vacuum (0.05-0.1 MPa), and concentrated under reduced pressure at about 30°C to obtain 6.9 grams of crude tanshinone.
[0037] Take a glass chromatographic column with a column length of 450 mm and an inner diameter of 45 mm, and install 350 ml of D101 macroporous adsorption resin, load the crude tanshinone above on the top of the chromatographic column, and then use mobile phases of 50%, 60%, and 70%, 80%, 90% ethanol-water solution for gradient elution, TLC plate tracking, concentration under vacuum (-0.6-0.1MPa), and water with absolut...
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