Preparation method of high-purity salvianolic acid A
A salvianolic acid, high-purity technology, applied in the field of preparation of high-purity salvianolic acid A, can solve the problems of decreased growth, increased dead seedling rate, decreased number of roots, diameter and length, etc.
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Embodiment 1
[0063] Example 1. (Taking 2000g comfrey as an example)
[0064] 1. Extraction: Weigh 2000g of comfrey (root and stem slices), heat and extract with 10 times the amount of water (20000ml) at 80°C for 2 hours, extract twice, combine and filter to obtain the extract.
[0065] 2. Transformation: Concentrate the extract to 4000ml, adjust the pH to 3 with 2mol / L hydrochloric acid, reflux for 7hr, and stop the reaction to obtain a transformation solution containing high-concentration salvianolic acid A.
[0066] 3. Separation: Weigh 2000g of DM301 macroporous resin, pretreat and pack into a column. Add the conversion liquid to the top of the chromatography column so that it completely enters the column bed. 5 column volumes were eluted with water to remove impurities, and then 3 column volumes were eluted with a solvent containing 70% ethanol, and these eluates were combined to obtain fractions containing salvianolic acid A.
[0067] 4. Purification: Concentrate the fractions under...
Embodiment 2
[0069] Example 2. (Taking 2000g comfrey as an example)
[0070] 1. Extraction: Weigh 2000g of comfrey (root and stem slices), heat and extract with 10 times the amount of aqueous solution at 100°C for 2 hours, extract twice, combine and filter to obtain the extract.
[0071] 2. Transformation: Concentrate the extract to 4000ml, adjust the pH to 5 with 0.5mol / L sulfuric acid, reflux for 5hr, and stop the reaction.
[0072] 3. Separation: Weigh 2000g of 330-type macroporous resin, pretreat and pack into a column. Add the conversion liquid to the top of the chromatography column so that it completely enters the column bed. 5 column volumes were eluted with water to remove impurities, and then 4 column volumes were eluted with a solvent containing 50% ethanol, and these eluates were combined to obtain fractions containing salvianolic acid A.
[0073] 4. Purification: After the fractions were concentrated to an appropriate volume, they were prepared and purified with a polyamide ...
Embodiment 3
[0074] Example 3. (Taking 1000g of comfrey as an example)
[0075] 1. Extraction: Weigh 1000g of comfrey (root and stem slices), heat and extract with 10 times the amount of aqueous solution at 85°C for 2 hours, extract twice, combine and filter to obtain the extract.
[0076] 2. Transformation: Concentrate the extract to 2000ml, adjust the pH to 6 with 0.2mol / L nitric acid, reflux for 24hr, and stop the reaction.
[0077] 3. Separation: Weigh 1000g of CAD45 macroporous resin, and pack it into a column after pretreatment. Add the conversion liquid to the top of the chromatography column so that it completely enters the column bed. 5 column volumes were eluted with water to remove impurities, and then 3 column volumes were eluted with 60% methanol, and these eluates were combined to obtain fractions containing salvianolic acid A.
[0078] 4. Purification: After the fractions were concentrated to an appropriate volume, they were prepared and purified with a Sephadex LH-20 colu...
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