Method for preparing total flavones of bastardtoad flax
A technology of thymegrass and total flavonoids, applied in the field of traditional Chinese medicine preparation, can solve the problems of unclear effective parts and low content of total flavonoids, and achieve the effect of high yield and simple process
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example 1
[0018] Take the dried thyme herbal material, crush it through a 40-mesh sieve, weigh 25g, add 500ml of 70% ethanol, heat and reflux for 2 hours, filter, add 250ml of 70% ethanol to the dregs, reflux for 1 hour, filter to remove the residue, and combine The filtrate was allowed to stand for 12 hours, centrifuged at 4000 rpm for 10 minutes, the supernatant was taken, the ethanol was recovered under reduced pressure, and dried under reduced pressure at 40°C. Dissolve the crude extract with 60ml of 95% ethanol, add 20ml of 1% basic lead acetate aqueous solution dropwise while stirring, let stand for 0.5 hours, and precipitate; suction filter the precipitate to dryness, add 60ml of 95% ethanol to suspend, and add 5 drops while stirring. % Sodium carbonate aqueous solution 10ml, let stand for 0.5 hours, precipitate, filter, add dilute hydrochloric acid to the filtrate to adjust the PH value to neutral, recover ethanol under reduced pressure, add water to 60ml, add 120ml n-butanol, extra...
example 2
[0020] Take the dried thyme herb material, crush it through a 40-mesh sieve, weigh 5g, add 100ml of 70% ethanol, heat to reflux for 2 hours, filter, add 50ml of 70% ethanol to the dregs, reflux for 1 hour, filter to remove the residue, and combine the filtrate ,Stand for 12 hours, centrifuge at 4000 rpm for 10 minutes, take the supernatant, recover ethanol under reduced pressure, add water to the remaining liquid to 50ml, place 100g on the HZ-80 macroporous adsorption resin chromatography column, after adsorption , Add distilled water to rinse until the effluent is colorless, then rinse the column with 60% ethanol, 10ml / min, until the effluent is free of flavonoid reaction. The above 60% ethanol effluents were combined, ethanol was recovered under reduced pressure, and dried under reduced pressure at 40° C. to obtain 0.235 g of brown-red powder with a yield of 4.7% (based on crude drug). Aluminum trichloride develops color, and its content is 19.7% determined by spectrophotometry....
example 3
[0022] Take the dried thyme herbal material, crush it through a 40-mesh sieve, weigh 10g, add 200ml of 70% ethanol, heat to reflux for 2 hours, filter, add 100ml of 70% ethanol to the dregs, reflux for 1 hour, filter to remove the residue, and combine the filtrate , Stand for 12 hours, centrifuge at 4000 rpm for 10 minutes, take the supernatant, recover the ethanol under reduced pressure, and dry under reduced pressure at 40°C to obtain 3.5 g of extract; add the crude thyme extract to 0.3 times column chromatography to polymerize Stir the amide powder evenly and dry at 50°C; after drying, the powder is placed on a polyamide resin chromatography column with 4 times the volume, rinsed with distilled water until the effluent is colorless, and then 30% ethanol, 50% ethanol and 70% ethanol, 10ml / min flush the column, while using thymusin I, thymusin II and thymusin III as the reference materials, thin layer chromatography to detect the effluent components; combine the fractions contai...
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