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

Inactive Publication Date: 2014-03-26
NANJING HOPE PHARM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent (CN 1394870A) discloses a method for extracting tanshinone compounds from the traditional Chinese medicine Salvia miltiorrhiza by high-speed countercurrent chromatography (HSCCC); The total tanshinone compounds were extracted and purified from the tra...

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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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PUM

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Abstract

The invention discloses a preparation method for extracting and purifying tanshinone monomeric compounds from red sage root. The method comprises the steps: washing the red sage root by using water, smashing, carrying out multi-stage counter current extraction by using an alcohol-acid solution, carrying out column chromatography by using macroporous resin, carrying out gradient elution by using an ethanol-water solution, collecting the eluent, evaporating and concentrating the eluent at reduced pressure and carrying out vacuum drying to obtain effective components tanshinone I, tanshinone IIA and cryptotanshinone. The method disclosed by the invention has the advantages that the multi-stage counter current extraction is carried out by using the alcohol-acid solution, the macroporous resin is reusable and the ethanol-water solution serves as the solvent, so that the method is economical and practical, high-purity tanshinone I, tanshinone IIA and cryptotanshinone monomeric compounds can be conveniently and efficiently obtained and the purity of the monomeric compounds is up to more than 95%; and the method is simple in process, simple and convenient in operation and low in cost and is suitable for volume production.

Description

technical field [0001] The invention belongs to the field of traditional Chinese medicine phytochemistry, and specifically relates to a preparation method for extracting and purifying tanshinone I, tanshinone IIA and cryptotanshinone monomer compounds from the traditional Chinese medicine Salvia miltiorrhiza. Background technique [0002] Salvia miltiorrhiza is also known as red ginseng, purple salvia miltiorrhiza, red root and so on. For Labiatae Danshen ( Salvia miltiorrhiza Bunge ) dry roots and rhizomes. First recorded in "Shen Nong's Materia Medica", it tastes bitter, slightly cold, and non-toxic. GUIXIN, Liver Channel. It has the effects of promoting blood circulation and regulating menstruation, dispelling blood stasis and relieving pain, cooling blood and eliminating carbuncle, clearing heart and eliminating troubles, nourishing blood and calming nerves, etc. It is mainly used in clinical treatment of diseases such as cardiovascular, hypertension, and cerebral isc...

Claims

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Application Information

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IPC IPC(8): C07J73/00C07J75/00
Inventor 徐德锋
Owner NANJING HOPE PHARM
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