Preparation method of active components in root-bark tree peony by in-phase leaching and sub-item preparation
A technology of paeonol extraction and extraction, which is applied in the field of extracting active ingredients in Chinese herbal medicine, can solve the problems of outdated and cumbersome technical means, waste of raw paeonol, and low production efficiency, and achieve the effects of reducing costs, reducing reagent consumption, and low cost
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Embodiment 1
[0028] Take 500g of paeonol crude drug, wash and dry, add 5L of water, and extract with warm water at 35°C for 8 hours. Filter to obtain medicinal residues and extracts. The extract (filtrate) uses an ultrafiltration membrane with a molecular weight cut-off of 10kDa, and is separated by tangential flow ultrafiltration at a pressure of 30psi and a temperature of 35°C to obtain a retentate containing the macromolecular paeonol polysaccharide and a permeate containing the small molecule total paeonol glycosides. over liquid. The paeonol polysaccharide retentate was precipitated with 3 times the volume of 70% ethanol for 12 hours, and the precipitate was collected and freeze-dried to obtain the paeonol polysaccharide fraction. The total paeoniflorin permeate liquid is concentrated under reduced pressure, the distillate is retained, the concentrated liquid is put on the macroporous resin column AB-8 (3.5g paeoniflorin / kg wet resin), and first washed with water for 6 column volumes...
Embodiment 2
[0030]Take 500g of paeonol crude drug, wash and dry, add 5L of water, and extract with warm water at 35°C for 8 hours. Filter to obtain medicinal residues and extracts. The extract (filtrate) uses an ultrafiltration membrane with a molecular weight cut-off of 30kDa, and is separated by tangential flow ultrafiltration at a pressure of 25psi and a temperature of 30°C to obtain the retentate containing the macromolecular paeonol polysaccharide and the permeate containing the small molecule total paeonol glycosides. over liquid. The paeonol polysaccharide retentate was precipitated with 3 times the volume of 80% ethanol for 12 hours, and the precipitate was collected and freeze-dried to obtain the paeonol polysaccharide fraction. The paeony total glycosides permeated liquid was concentrated under reduced pressure and then applied to the macroporous resin column AB-8 (3.5 mg paeoniflorin / g wet resin). First, rinse 6BV with water to remove impurities, then elute 3BV with 50% ethano...
Embodiment 3
[0032] (1) The mensuration of paeonol purity in embodiment one (ultraviolet detection-high performance liquid chromatography)
[0033] Chromatographic conditions: column Restek pinnacle C 18 Column (4.6 * 250mm, 5 μ m); Detector Waters2487 ultraviolet detector (U.S. Waters Company); Waters515 chromatography pump (U.S. Waters Company); Detection wavelength 274nm; Mobile phase methanol: water=45:55 (v / v); 1mL / min; injection volume 20μL.
[0034] Preparation of the test solution: Accurately weigh an appropriate amount of the paeonol sample and standard substance in Example 1 of the same quality, dissolve them in a volumetric flask with methanol, shake well, and obtain.
[0035] Determination method: Precisely draw sample solution and standard solution respectively, inject liquid chromatograph, calculate and measure by peak area normalization method, see results figure 2 .
[0036] Analysis results: figure 2 Among them, the relative retention time of the paeonol peak was 14....
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