Preparation method for total flavonoids in V.amoena Fisch.var.angusta Freyn.
A technology of vetch and total flavonoids, applied to medical preparations containing active ingredients, pharmaceutical formulas, non-central analgesics, etc., can solve the problem of low extraction rate, achieve high extraction rate, high physical stability, and adsorption good selectivity
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Embodiment 1
[0012] The preparation method of embodiment 1 total flavonoids of wild pea
[0013] 1) Extraction: take 10 g of the medicinal material powder of Vetchia sayama, 200 mL of 70% ethanol aqueous solution (the ratio of liquid to material is 1:20), and the extraction temperature is 90 ° C, and the extraction is performed twice, and the extraction time is 1 hour each time to obtain the extract;
[0014] 2) Purification: Select an adsorption column (Φ1.5cm×20cm, 10g) filled with HPD-826 macroporous adsorption resin, and rotatively evaporate the extract obtained in step 1) to recover ethanol to obtain a concentrated solution, and add water to the concentrated solution to adjust the concentration 0.39mg / mL, use HCl to adjust the pH of the sample aqueous solution to 5.5, the loading volume is 5 times the volume of the resin column bed, and the flow rate is adjusted to 2mL / min for dynamic adsorption. The eluent is 70% ethanol aqueous solution, and the flow rate is 3mL / min Carry out elutio...
Embodiment 2
[0016] The optimization of embodiment 2 extraction steps
[0017] (1) The influence of extraction solvent
[0018] Accurately weigh 5g of the wild pea medicinal material powder (No. 4 sieve), totally 7 parts, put in a 250ml Erlenmeyer flask, add 40%, 50%, 60%, 70%, 80%, 95% ethanol aqueous solution 75ml respectively (material The liquid ratio is 1:15), heated at 90°C for 1 hour, and extracted twice. The extracts were combined, evaporated to dryness, dissolved in methanol, and adjusted to 50ml. Determination of the content of total flavonoids in the extract, the results are shown in Table 1.
[0019] Table 1 Extraction Reagent Investigation Results
[0020]
[0021] (2) The influence of extraction conditions
[0022] The extraction solvent concentration is 70% ethanol aqueous solution. Orthogonal experimental design was carried out with four factors: extraction temperature, solid-liquid ratio, extraction time, and extraction times. The factor levels are shown in Table 2,...
Embodiment 3
[0030] The optimization of embodiment 3 purification steps
[0031] (1) The effect of macroporous adsorption resin on the total flavonoids of Sayama vetch
[0032] The resin models investigated are HPD-750, HPD-600, HPD-826, HPD-5000, ADS-17, ADS-7, AB-8, D101, X-5, DM-130. Accurately weigh 1 g of each of the 10 pretreated macroporous resins (dry and anhydrous), place them in a 50 mL Erlenmeyer flask, and add 50 mL of crude drug concentration of 0.17 g / mL solution (5 kinds of flavonoid glycoside concentration C 0 0.6404mg / mL), shake constantly (120r / min), shake for 2 hours, filter, take the filtrate, measure the content of 5 flavonoid glycosides, and get the concentration C 1 . Take the 10 kinds of macroporous resins obtained by the above filtration, place them in 50mL conical flasks respectively, add 50mL70% ethanol aqueous solution respectively, shake from time to time (120r / min), shake for 2 hours, filter, take the subsequent filtrate, measure The content of 5 flavonoid ...
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