Method for purifying salvianolic acid A by using reversed-phase chromatography
A technique of salvianolic acid and reversed-phase chromatography is applied in the field of purifying salvianolic acid A, which can solve the problems such as inability to widely use salvianolic acid A for batch preparation, small sample loading, limited pH range, etc., and achieve stable and controllable product quality. , Reduce the separation load, the cost is acceptable
Inactive Publication Date: 2011-10-12
YANTAI TARGET DRUG RES +1
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Problems solved by technology
[0008] Traditional C 18 Reversed-phase chromatography cannot be widely used due to factors such as small sample volume, limited pH range, inability to perform effective regeneration, short life, and cost constraints.
The reversed-phase resin fillers developed in recent years have not been able to effectively solve this problem, so that reversed-phase chromatography cannot be widely used in the batch preparation of salvianolic acid A
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Embodiment 1
[0050] Crude product of salvianolic acid A (502 grams, content 81.7%)→dissolved in water (10mg SA / mL, pH 3.0, 41L)→CG161S reversed-phase resin column (Φ200×500, column bed height 15cm)→20% acidic ethanol ( pH 3.0) until pure SA appears before elution (collect the eluate according to the column volume → HPLC quantitative, TLC qualitative detection and combined concentration and drying → section A) → 40% alcohol solution is eluted to a small amount of SA (collect the eluate according to the column volume Deliquification→HPLC quantification, TLC qualitative detection and combined concentration and drying→B section)→60% alcohol solution to elute residual SA to no SA (collect the eluate according to column volume→HPLC quantification, TLC qualitative detection and combined concentration and drying→C part). Total weight 346.5 grams, salvianolic acid A 328.1 grams, content 94.7%, yield 80%.
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The invention provides a method for purifying salvianolic acid A by using reversed-phase chromatography based on physical and chemical properties and chromatograph behavior of a chemical component in salvia miltiorrhiza as well as adaptability of salvia miltiorrhiza to a cell separation technology. In the method, a used reversed-phase chromatography filling material is reversed-phase resin CG161, SBC-MCI-GEL or MCI-GEL-CHP-20P, and the weight ratio of salvianolic acid A to used the reversed-phase chromatography filling material is 1: (30-50); and the reversed-phase chromatography is operated by the following steps: sampling a crude salvianolic acid A aqueous solution; eluting with a 20%-25% alcohol solution until the salvianolic acid A is detected in eluent; eluting with a 35%-40% alcohol solution and collecting salvianolic acid A until the content of salvianolic acid A in eluent is minimum; and finally, eluting with a 50-70% alcohol solution and collecting salvianolic acid A containing impurities. The product prepared by the method is stable and controllable in quality and is acceptable in cost.
Description
technical field [0001] The invention relates to a method for purifying salvianolic acid A by reverse 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, d...
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IPC IPC(8): C07C69/732C07C67/56B01D15/42
Inventor 何克江刘珂韩飞陈栋刘军锋张祁
Owner YANTAI TARGET DRUG RES
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