Salvia minium phenolic acid A and process of preparing preparation and use
A technology of salvianolic acid and salvianolic acid, applied in the field of medicine, can solve the problems of high requirements for purified samples, high cost of reversed-phase silica gel, and low yield of salvianolic acid A, etc.
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Embodiment 1
[0202] Embodiment one: the preparation method of salvianolic acid A, its processing step is:
[0203] 1. Take 100kg of Danshen crude powder, add 8 times the amount of 70% ethanol to reflux and extract 3 times, each time for 1.0 hour, and filter;
[0204] 2. Concentrate the combined filtrate to medicinal material: medicinal liquid (1:4), adjust the pH value of the concentrated solution to 6.0, place it in a reaction tank at 110°C, and have a gauge pressure of 0.05MPa, and react for 6 hours;
[0205] Gauge pressure 0.05MPa, reaction for 6 hours;
[0206] 3. Filter the reaction solution, pass the filtrate through the AB-8 type (manufactured by Nankai University Chemical Factory) macroporous adsorption resin column (the amount of medicinal material: resin is 1:2), wash with water until the sugar detection reaction is negative, and then use 10% ethanol Eluted to FeCl 3 If the reaction is negative, then elute with 30% ethanol, use HPLC to track and detect, collect the eluate conta...
Embodiment 2
[0210] Embodiment two: basically the same as embodiment one, the difference is that in step 3, the macroporous resin model is changed to HPD-100 (produced by Cangzhou Baoen Chemical Co., Ltd.); Amide chromatography column (medicine material: resin ratio: 1:2), wash with water until the sugar detection reaction is negative, then use 40% ethanol to elute to FeCl 3 If the reaction is negative, it is eluted with 80% ethanol, followed by high performance liquid phase detection, and the eluate containing salvianolic acid A is collected and concentrated under reduced pressure until there is no organic solvent; in step 5, the pH value is adjusted to 5.
[0211] It was determined that the content of salvianolic acid A was 97.97, the retention time of salvianolic acid A was 45.44 minutes, the retention time of impurity 1 was 32.14 minutes, the relative retention time of impurity 1 was 0.707, the content of impurity 1 was 0.57; the retention time of impurity 2 was 61.78 minutes, and the r...
Embodiment 3
[0212] Embodiment three: basically the same as embodiment one, the difference is that the macroporous resin in step 3 is changed to HPD-300 (produced by Cangzhou Baoen Chemical Co., Ltd.); step 4 is changed to filter the concentrated solution, and the polyamide layer on the filtrate Analyze the column (the amount of medicinal material: resin is 1:2), first wash with water until the sugar detection reaction is negative, then use 50% ethanol to elute until salvianolic acid A appears in the eluent, then elute with 95% ethanol, and use High-performance liquid phase tracking detection, collecting the eluate containing salvianolic acid A, and concentrating under reduced pressure until there is no organic solvent.
[0213] It was determined that the content of salvianolic acid A was 97.87, the retention time of salvianolic acid A was 45.594 minutes, the retention time of impurity 1 was 32.27 minutes, the relative retention time of impurity 1 was 0.708, the content of impurity 1 was 0....
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