Method for preparing specnuezhenide
A technology of privet privet and privet privet, which is applied in the field of high-purity privet privet, and can solve problems such as complex processes and operations, and unsuitability for large-scale preparation of pure privet privet
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Embodiment 1
[0021] Take 10kg of Ligustrum lucidum medicinal material, pulverize it, add 10 times, 8 times, and 8 times the amount of medicinal material to decoct 3 times, decoct for 2 hours each time, filter each time and combine the filtrate, and the filtrate is properly concentrated; the concentrated solution is sampled in On the D-101 macroporous resin column, first elute with water, discard the washing liquid, then elute with 20% ethanol, collect the eluate, concentrate to a liquid extract; add methanol to stir fully, place the precipitate, filter, The filtrate was evaporated to dryness; finally separated and purified with a normal phase silica gel column and a reverse silica gel column to obtain about 28g of a compound with a purity of 98%, combined with the NMR identification results and existing literature research spectrum data, it was determined that the compound was Privet privet Glycosides.
Embodiment 2
[0023] Take Ligustrum lucidum medicinal material, crush it; weigh 203g, add 400ml of water to soak for 30min, then add 1200ml of water to extract for 2h, filter, then add 1600ml of water to extract twice, filter, combine the three filtrates, and concentrate the filtrate to about 400ml; load the sample on D- 101 macroporous resin column, first eluted with water, discarded the water eluent, then eluted with 40% ethanol, and the eluate was concentrated to a liquid extract (about 40ml); add industrial alcohol (95% ethanol) 200ml, Fully stirred and shaken, left to precipitate for 2 hours, filtered, and the filtrate was evaporated to dryness; then purified with a normal phase silica gel chromatography column to obtain 3.375 g of the crude product of teruci, with a purity of 81.18%, and the yield at this time was 63.61%. Purified by reverse silica gel column chromatography, 1.440 g of pure privetin was obtained, with a purity of 98.13%, and a yield of 21.55%.
Embodiment 3
[0025] According to the method for preparing privetin according to the patent CN101704857A, take 227g of the pulverized privet privet medicinal material, purify it to obtain 1.853g of pure privet, and its content is 98.40% as measured by HPLC. At this time, the yield of privet was 20.03%. By comparison, it is found that the yield of the invention patent CN101704857A for preparing terucitoside is slightly lower than that of the patented method. Example 2 produced 1.440g of pure privetin, with a purity of 98.13%, and its cost was calculated at 799.3 yuan / g with reference to the prices of various reagents and materials purchased in the laboratory; the patent CN101704857A preparation method produced pure privetin Product 1.853g, content is 98.40%, and the calculation cost with the cost calculation method of embodiment two is 925.0 yuan / g. When the dosage is increased to 100kg, the cost is further reduced, combined with further reasonable calculation and calculation of the market ...
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