Method for separating and purifying salvianolic acid from red sage root liquid extract by one step

A technology of separation and purification and water extraction, which is applied in the separation/purification of carboxylic acid compounds, medical preparations containing active ingredients, organic chemistry, etc. It can solve the problems of unreported parameters such as purity and yield, and unclear structure-activity relationship. And other issues

Inactive Publication Date: 2008-05-28
TIANJIN UNIV
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Problems solved by technology

[0004] At present, the water-soluble components of Salvia Miltiorrhiza are mostly obtained by methods such as water extraction, alcohol precipitation, and ethyl acetate extraction. Literature (Chinese Patent Medicine, 2007, 29(1): 143-144; Chinese Herbal Medicine, 2007, 38(6): 843-846 ; Chinese Herbal Medicine, 2007, 38 (4): 542-545; Shi Zhen Guoyi Guoyao, 2007, 18 (5): 1186-1187) are all elaborated in detail, but the resulting product may be a mixture of polyphenolic acids, and the structure-activity relationship is not Clear; or after multi-step purification to obtain a single medicinal substance, such as CN1342638A adopts water extraction-double column adsorption elution-solvent extraction and other steps to purify Danshensu, CN1303052C adopts water or alcohol extraction-precursor conversion-ultrafiltration to remove Miscellaneous-solvent extraction-normal phase chromatography and other multi-step purification of Danshensu, CN1751706A adopts alkali extraction-acidification-alcohol precipitation-double column (resin+polyamide)

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  • Method for separating and purifying salvianolic acid from red sage root liquid extract by one step

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Embodiment 1

[0027] (1) Water extraction and alcohol precipitation: Take Danshen medicinal material and crush it to 20-35 meshes, extract with 15 times of water, add 95% ethanol to make the ethanol volume content in the extract reach 60%, refrigerate at 4°C for 24 hours, and then centrifuge. 5500 revolutions per minute, recover the supernatant, and spin-steam until ethanol-free to obtain the water-extracted ethanol-precipitated liquid of Salvia miltiorrhiza.

[0028] (2) Acidification and salt addition: Take 200 milliliters of the water-extracted alcohol sedimentation solution and adjust the pH to 3.5 with 4% hydrochloric acid (mass concentration), remove the flocculent precipitate by centrifugal filtration, and add 4 g of sodium chloride at a rotating speed of 5500 rpm.

[0029] (3) Loading and elution: the above-mentioned extracted solution flows through a resin with a diameter of 19 mm at a flow rate of 1.33 times the volume of the resin per hour at 25°C, with a length-to-diameter ratio ...

Embodiment 2

[0033] (1) Water extraction: take Danshen medicinal material and crush to 20-35 mesh, and extract with 15 times of water.

[0034] (2) Acidification and salt addition: take 200 ml of water extract and adjust the pH to 3.5 with 4% hydrochloric acid (mass concentration), centrifuge and filter to remove flocculent precipitates, the rotating speed is 5500 rpm, and then add 4g of sodium chloride.

[0035] (3) Loading and elution: the above-mentioned extracted solution flows through a resin with a diameter of 19 mm at a flow rate of 1.33 times the volume of the resin per hour at 25°C, with a length-to-diameter ratio of 1:10, and filled with weakly polar large resins. Pore ​​adsorption resin SP825 chromatographic column for dynamic adsorption; after loading the sample, use 250 milliliters of distilled water to carry out dynamic elution with a flow rate of 1.33 times the resin volume / hour, and collect the water eluate; then use distilled water and 95% ethanol The mixed solution (the v...

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Abstract

The invention relates to a method for furthering separating and purifying salvianolic acid from Danshen extract fluid, which comprises that prepares, breaks and extracts Danshen via water solution, acidifies extract to adjust pH and adds salt to process post-treatment, processes dynamic continuous adsorption and elution on the treated extract at chromatography column stuffed with resin adsorbent, elutes via water, collects and concentrates eluent, elutes via gradient ethanol solution, segmented collects and concentrates eluent, and dries the concentrates solution to obtain product. The invention can simply, effectively and quickly separate and purify various salvianolic acids, wherein test on different salvianolic acid products shows that the highest yields of tanshinol, alkannic acid, rosmarinic acid, salvianolic acid A and salvianolic acid B are 35. 55%, 70.65%, 99.27%, 82.78%, and 89.34%, and relative highest purities are 95.32%, 65.05%, 29.40%, 33.93%, and 82.35%, which are near or higher than the result of purification on the goal of single component.

Description

technical field [0001] The present invention relates to extraction technology of functional components of natural plants, especially a method for one-step separation and purification of salvianolic acid from water extract of salvia miltiorrhiza Methods. Background technique [0002] Salvia (Salvia miltiorrhiza Bunge) is a perennial herb belonging to the genus Salvia of the Labiatae family. Its dry root is a traditional Chinese medicine that has a long history of promoting blood circulation and removing stasis. Blood, promoting blood circulation and removing blood stasis, nourishing blood and nourishing Qi, dispelling numbness and strengthening feet, regulating menstruation and stopping collapse, detoxification and expulsion of pus". [0003] The water-soluble components of Danshen have a wide range of pharmacological effects, such as protecting myocardial ischemia and hypoxia, improving microcirculation, central sedation, inhibiting platelet aggregation and thrombus formati...

Claims

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Application Information

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IPC IPC(8): C07C59/52C07C51/42C07D307/80A61K36/53
Inventor 齐崴何志敏吴小东王红蕾
Owner TIANJIN UNIV
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