The extraction methods of Cardamom Cloves mainly include ethanol extraction, ether extraction, acetone extraction, chloroform extraction, etc., and silica gel column chromatography is used. Cardamomine obtained by these extraction and separation methods has low content, low yield and long extraction time, and is generally used as a small amount of preparation method in chemical composition research laboratories. Shi Daohua etc. impregnated with 95% ethanol for 3 days, refluxed 2 times with 8 times the amount of ethanol, 2 hours each time, recovered the ethanol under reduced pressure to obtain 600ml concentrated solution, made the concentrated solution into an aqueous suspension, and then used ethyl acetate, n-butanol Sequential extraction, the extract was decompressed to recover the solvent, concentrated to obtain 340g of extract, the extract was dissolved in an appropriate amount of acetone, the sample was mixed, and the column was wet-packed with silica gel equivalent to 5 times the amount of the solid, and eluted with petroleum ether-ethyl acetate system , collect the eluted fractions, spot on the same thin-layer plate as the reference substance, develop with toluene-ethyl acetate-methanol (15:4:1), chloroform-methanol (20:1) respectively, and UV light Observe under (wavelength 365nm), merge the fraction that appears dark spot in the corresponding position of reference substance, concentrate at normal pressure to obtain 13g mixed crystal. The mixed crystals were passed through a silica gel column, and the eluent was petroleum ether-ethyl acetate-acetone system. After concentration, 5 g of crystals were obtained. Take 100g of gel to swell overnight with methanol, put it on the column, dissolve the crystals in methanol, take 20ml and put it on the column, collect 3ml of each part, analyze by thin layer (TLC) and compare with the standard, combine the same fractions and concentrate to get orange needles Although this method has significantly improved than the acetone extraction method, the extraction rate is 0.084%, but the extraction rate is still very low, the extraction time is long, the organic solvent extraction extraction rate is low, and the loss is large.
CN201010235806.0 provides a method for extracting Cardamom Cloves with high extraction rate, short cycle and high purity.
Technical solution: In order to achieve the above object, the present invention provides a method for extracting Cardamom Cloves from Cardamom, which specifically includes the following steps: a. Extraction step: take an appropriate amount of Cardamom seeds, crush them to 20-60 mesh, and use cold infiltration , warm soaking or reflux extraction method, the cardamom seed powder is extracted with solvent for 1-3 times, the extracts are combined, concentrated under reduced pressure to obtain the extract; b. Organic solvent extraction step: extract the extract with petroleum ether until the extract is close to Colorless, discard the petroleum ether extract, keep the remaining extract; c. Separation and purification step: use column chromatography to separate the remaining extract, use water, methanol, ethanol, ethyl acetate, acetone, dichloromethane or their mixture The solution is eluted, monitored by high-performance liquid chromatography, and the effluent containing Cardamom Cloves is collected. After the effluent is concentrated, it is crystallized with an organic solvent to obtain high-purity cardamomine. Compared with the prior art, the extraction method of Cardamom Cloves provided by the method has the following advantages: (1) the route design of the method provided by the invention is reasonable, and the method is simple and easy to operate; (2) the method period provided by the invention is short and the extraction rate is high , the product has high purity; (3) the solvent used in the method provided by the invention and the column chromatography filler can all be recycled and recycled, which can reduce costs, and is a low-cost, cyclic process.
