Method for preparing methanoquinone from henna
A technology of manna quinone and henna, which is applied in the field of extracting and separating active ingredients manna quinone and naphthoquinone, can solve the problems of cumbersome operation, large organic solvent, and unsuitability for large-scale production, and achieve simple process and high effect Good, the effect of reducing the heating temperature
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[0029] In the method for preparing menaquinone, the extraction reagent used is an aqueous solution of sodium hydroxide, sodium bicarbonate, potassium hydroxide, sodium bicarbonate or a mixture thereof, and the pH value of the extraction reagent is 7.0 to 13.2, preferably 12.7 ~13.1, adopt the method of ultrasonic extraction, the ultrasonic extraction temperature is 10~70°C, the optimum is 15~45°C, the ultrasonic extraction time is 30~90min, the optimum is 45~75min, the ultrasonic power is 50~800W, the optimum It is 100~150W.
[0030] According to the method for preparing menaquinone, the extraction solution obtained under optimal conditions is analyzed by ultraviolet spectrophotometry at 460 nm, and the extraction rate of megenone can reach 3% or above.
[0031] The method for preparing menaquinone uses a macroporous resin dynamic adsorption-elution method, the macroporous adsorption resin is non-polar or weakly polar, and the three elution solvents are water, 20% to 30% ethan...
Embodiment 1
[0037] (1) Take 100g of henna peel and leaf powder as raw materials, add 800ml of water, shake and mix well, soak for 12h, and then 30℃100W ultrasonic extraction for 30min. Centrifuge and filter to obtain the extract, then repeat the above steps to extract the raw material twice, and combine the two extracts.
[0038] (2) Add the extract obtained in the above steps into NK-9 macroporous adsorption resin with a volume of 1500ml, control the flow rate so that the solution flows slowly through the macroporous resin, and the galenone in the extract is adsorbed on the macroporous adsorption resin. resin. The macroporous adsorption resin was eluted with 5000ml water, 4000ml30% ethanol aqueous solution and 4000ml60% ethanol aqueous solution successively.
[0039] (3) Remove ethanol from the 60% ethanol eluate obtained in the above steps with a vacuum solvent recovery device, set the heating temperature at 40°C, concentrate until the remaining solution volume is 1000ml, make dry powd...
Embodiment 2
[0042] (1) Take 10g of henna peel and leaf powder as raw materials, add 100ml of sodium hydroxide solution with a pH of 13, shake and mix well, soak for 0.5h, and then 30°C 100W ultrasonic extraction for 30min. Centrifuge and filter to obtain the extract, and adjust the pH to be neutral.
[0043] (2) Add the extract obtained in the above steps into the AB-8 macroporous adsorption resin with a volume of 200ml, control the flow rate, so that the solution flows slowly through the macroporous resin, and the methine in the extract is adsorbed on the macroporous adsorption resin. resin. The macroporous adsorption resin was eluted with 600ml of water, 500ml of 30% ethanol aqueous solution, and 500ml of 70% ethanol aqueous solution in sequence.
[0044] (3) Remove ethanol from the 70% ethanol eluate obtained in the above steps with a vacuum solvent recovery device, set the heating temperature at 45°C, concentrate until the remaining solution volume is 150ml, make dry powder with a fr...
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