Extraction and isolation of palm leaf anthemisine and preparation of fenugreek ethanol
Extraction and isolation of palm leaf anthemisine and preparation of fenugreek ethanol
Extraction and isolation of palmarosa anthelmintic alkaloids and experiments on the preparation of yanhuisuo ethanol can be used for: utilizing it to alleviate pain caused by disorders of the gastric system, prodromal paroxysms, headache, insomnia, and so on.
Operation method
solubility difference method
Principle
After the hydrogenation of the palm-leaf anthemisine, it is the analgesic and sedative drug Yanhuisuo ethylin (Tetraydropalmatine), and the content of Yanhuisuo ethylin in the traditional Chinese medicine Yanhuisuo is very low, so Huangteng has become the main raw material of the palm-leaf anthemisine and the Yanhuisuo ethylin in the industrial production.
Materials and Instruments
Huangteng crude powder Move 1, leaching: take 100g of Huangtian crude powder, with 1% acetic acid cold immersion (to submerge the degree of raw materials, about 500ml) 1-2 days, nylon cloth filtration, dregs of the cold immersion of 15 acetic acid for one day, combined with the filtrate (retained 1ml for the alkaloid qualitative reaction). 2, salt precipitation, neutralization: filtrate with 40% NaOH solution adjusted to pH9 at the same time add 7% refined salt, that is, there is a yellow insoluble material precipitation, 80 ℃ insulation, so that the precipitation cohesion, static, pouring out the upper layer of clear liquid, filtered through a chrysanthemum-shaped filter paper, to get the parmesan free alkali crude products, drying. 3, refining: the crude parmesan, add 80% ethanol 100ml, heating reflux to dissolve, about ten minutes, multiply the heat of filtration, the residue and then add a small amount of ethanol with the method of treatment, filtration and finally take ethanol with a dropper to wash the insoluble material on the Buchholz funnel, combined with the filtrate and filtrate dropwise addition of 6N hydrochloric acid to the filtrate to the PH2 placed, that is, there are golden-yellow needle crystals precipitation, filtration, and then recrystallized from ethanol, method, the chloride of parmesan crude crystals placed in a triangular burner, and the method, will be chlorinated. Bamartine chloride crude crystals placed in a triangular flask, using a dropper to add 95% ethanol so that the crystals just dissolved (heated on a water bath), filtration to obtain a clarified solution, stoppered to place the precipitation of crystals. If the filtrate has precipitated crystals in the filtration, it can be heated in water on the crystallization of fully soluble and then add the stopper placed, so that the precipitation of the crystal shape is good. If the volume of filtrate is too large, can be dissolved to the bottle wall edges slightly solid when added to the plug crystalization. The mother liquor is properly concentrated, and can precipitate a part of Palmatine chloride. 4, reduction: take 1g of Palmatine chloride refined products, put 50-100ml garden bottom flask with distilled water 10ml, 0.5ml of concentrated sulfuric acid, zinc 0.7g (industrial production should be added in batches of zinc powder), direct heating to keep boiling, the reaction for 4-5 hours (the reaction process and the color of the solution gradually fade until colorless), the reaction is complete, pour out the upper layer of the clear liquid, and then a little distilled water (1-2ml) slightly heated to wash the reaction flask. 2ml) slightly heated to wash the reaction bottle and zinc residue 1-2 times, the combined solution is cooled that there is Yanhusuo ethyl acid sulfate precipitation. Filter, take the crystals in a 25ml conical flask, with 70% ethanol 10ml heating to dissolve. Filtering while hot, and then a small amount of ethanol (1-2 ml) to wash the container, to the hot solution (about 60 ℃) in drops of ammonia to PH9, immediately precipitated scaly crystals, filtration, washed with distilled water (the resulting crystals can be dissolved with water? Can it be dissolved by adding chloroform?) Dried to obtain free base of yanhuisu ethanol. Drying. 5, into the salt: weigh 0.5 g of free base of Yanhuosu ethin. Placed in a 25 ml conical flask (or a small flask) with 90% ethanol 4 ml, heating on a water bath to dissolve, with a coarse capillary drops of 5% ethanol sulfate solution to Congo red paper was light blue (PH about 5) cooling precipitation crystals. Will be slightly yellow columnar crystals, filtered dry below 50 ℃ dry, that is, Yanhuosuo ethanol neutral sulfate. Can be recrystallized with water once, after drying to measure the melting point. Extracted with acetic acid water small samples, the general rate of 1-2%, with ethanol reflux leaching rate of 3-4%, take 100g of Huangteng crude powder, with 95% ethanol reflux leaching for three or four times combined with ethanol to about 120 ml, can be refined according to the third step under the operation, add hydrochloric acid to get barmartine chloride. Caveat 1, Huangteng contains polysaccharide substances dissolved in water, often affecting the salting out of the water solution and neutralization and filtration, so it is appropriate to pour most of the clarified liquid after static and then filtered with a cloth bag to collect the precipitate, the raw materials should not be crushed too fine. 2， Palmatine chloride is golden needle-like crystals, and has a strong yellow fluorescence. Tetrachloropalmatine for the first colorless flaky crystals, do not have fluorescent. Therefore, the color of the reaction solution can be used as a judgment of the reduction endpoint. At the beginning of reduction, the reaction liquid is orange-yellow, with the reduction reaction, the reaction liquid color gradually recede, to light beige or colorless can be used as the end point of the reaction. 3、Tetrahydropalmatine is easy to be oxidized to palmatine, so it should be operated continuously as soon as possible in the preparation process. 4， tetrahydropalmatine hydrochloride and acid sulfate in water solubility is small, so generally made of water-soluble neutral sulfate, for the preparation of injections. Common Problems In this experiment, the content of the alkaloid was compared with different concentrations of aqueous sulfuric acid and glacial acetic acid, different maceration times, different alkali concentrations, and different amounts of sodium chloride, and the results showed that 20 mL/L of glacial acetic acid, macerated for 24 h, alkalized at pH 10.0, and 11 % sodium chloride were suitable for the extraction of alkaloid from Ribes nigrum. The results of this experiment can provide a basis for the actual production process of extracting palm-leaf anthemisine from Rhinophora japonica. For more product details, please visit Aladdin Scientific website.
Acetic acid Sodium hydroxide Sodium chloride Ethanol Hydrochloric acid Palmatine chloride Zinc powder Sulfuric acid Distilled water Chloroform Congo red paper
Nylon cloth, daisy filters, glass rods, distillation flasks, Brinell's funnels, water baths, microwaves, ovens, round-bottomed flasks, alcohol lamps, conical flasks, capillary tubes, filtering flasks.
Source: Exploration of the extraction conditions of the palm-leaf anthemisine from Ranunculus tataricus, Yanbian University Medical Journal, Research on the method of preparing ethanol from Ranunculus tataricus, World Science and Technology.