Separation method for simultaneously preparing five dopamine compounds from aspongopus
A separation method, the technology of Jiuxiangworm, applied in the separation/purification of carboxylic acid amide, organic chemistry, etc., can solve the problems of low yield, too many types of solvents, complicated technical solutions, etc., achieve high separation efficiency and prolong the use of instruments Cycle time, effect of reducing sample volume
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[0030] 1. Grind 1Kg of the dried chrysanthemum worm into a coarse powder of 1-5mm, add 5L of 70% ethanol solution, ultrasonically extract 3 times, the ultrasonic time is 60min, 45min, 30min, combine the extract 15L, filter, 60 °C and concentrated in vacuo to no purity, about 2L of solution. Add 800ml of petroleum ether, ethyl acetate, and n-butanol in sequence, extract each solvent 3 times, combine the n-butanol solution, about 2.5L, concentrate in vacuo at 60°C to 200ml, add 200g of 200-mesh silica gel to mix the sample, and perform a silica gel column Chromatography, chloroform-methanol gradient elution, collect 1 / 5-1 / 1 eluted fraction, concentrate to about 100ml, add 50ml of methanol, filter with 0.45μm organic membrane; inject the filtrate to prepare and separate the compound monomer, and Targeted collection of each component greater than 98.0%, combined the same fractions, during this process, the detection wavelength of the ultraviolet detector was set at 280nm, and comp...
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