Method for purifying salvianolic acid A by adopting normal phase chromatography
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A technology of salvianolic acid and normal phase chromatography, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as unsatisfactory effect, membrane pore blocking membrane life, loss of target compound, etc., and achieve product quality Stable and controllable, reduced separation load, acceptable cost effect
Inactive Publication Date: 2011-10-12
YANTAI TARGET DRUG RES +1
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[0010] Although membrane separation technology can effectively remove pseudo-colloidal impurities, because it is a non-tangential force separation technology, the target compound often has a very high affinity with this type of impurity, resulting in serious loss of the target compound
In addition, when membrane technology is used for the separation of such impurities, it also
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[0051] Salvianolic acid A crude product (94.7% SA, 346.5g) → dissolve in a small amount of ethyl acetate (about 800ml) → add 800g silica gel and mix well → dry under reduced pressure in a rotary evaporator to become a fluid powder (50°C) → silica gel wet Column (Φ100×1000, n-hexane prepacked with 1500g silica gel) → n-hexane / tert-butyl methyl ether (7 / 3) elution to SA detection (collect eluate according to column volume → HPLC quantitative, TLC qualitative detection and combined concentration Drying → Section A) → n-hexane / tert-butyl methyl ether (6 / 4) eluted to a small amount of SA (collect the eluate according to the column volume → HPLC quantification, TLC qualitative detection and combined concentration and drying → Section B) → n-hexane / tert-butyl methyl ether (5 / 5) was eluted until the eluate was colorless (collect the eluate according to the column volume→HPLC quantification, TLC qualitative detection and combined concentration and drying→section C). Section B has a to...
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Abstract
The invention provides a method for purifying salvianolic acid A by adopting a normal phase chromatography based on physicochemical properties, chromatographic behaviors and unit separation technology adaptabilities of chemical compositions of salvia miltiorrhiza. A normal phase chromatographic packing is chromatographic silica gel the granularity of which is 100-200 meshes, wherein the normal phase chromatography comprises the following operation steps of: extracting a salvianolic acid A aqueous solution by using ethyl acetate; concentrating ethyl acetate extract liquor until the solid content is 20-30 percent; adding chromatographic silica gel in an amount which is 2-2.5 times that of the salvianolic acid A; putting into a rotatory evaporator for drying at reduced pressure to obtain a flowing solid sample; and putting the solid sample at the top end of a silica gel wet column. A produced prepared with the method has stable and controllable quality and acceptable cost.
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technical field [0001] The invention relates to a method for purifying salvianolic acid A by normal phase chromatography. Background technique [0002] Salvia miltiorrhiza is the basic treatment drug for cardiovascular and cerebrovascular diseases in my country. Due to its definite curative effect, Danshen has become the traditional Chinese medicine with the largest consumption (15,000 tons / year), the highest sales, and the largest number of preparation factories in China (960 preparation factories, and the main dosage forms are: Danshen Dropping Pills, Danshen Injection, Danshen Tablets, Danshen Granules, Danshen Granules and Danshen Capsules), in addition, Danshen is also compounded with other medicinal materials for pulmonary heart disease, hyperlipidemia, hyperviscosity syndrome, asthma, bronchopneumonia, Hepatitis, liver cirrhosis, nephrotic syndrome, arthritis, diabetes, circulatory disorders, various bacterial and viral infections, anti-endotoxin, tumor, scleroderma, de...
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