Physical and chemical identification
1. Sublimation of traces of powder, fine acicular or granular crystals.
2. Take 1 ml each of the ephedra acid aqueous infusion, set them in 2 test tubes, and add 1 drop of potassium iodide bismuth iodide test solution into the tube to produce yellow precipitate; add 1 drop of mercury iodide and potassium chloride test solution to the tube without precipitation ( Check alkaloid).
3. Take an acid aqueous extract, after alkalinization, extract with diethyl ether, wipe away the ether, dissolve the residue with acid water, add a few drops of 0.5% copper sulfate test solution, add 10% sodium hydroxide solution to the purple color (copper-chromium salt), and then After adding a few ml of ether and shaking it, the ether layer was purple, and the water layer was blue (L-ephedrine biuret reaction).
4. TLC
(1) Ephedra
(2) Ephedra
(3) Ephedra
(4) Ephedrine Hydrochloride
Thin layer chromatography:
Sample solution: Take powder 1g, add water 15ml, reflux for 30 minutes, filtered. The filtrate was basified, extracted with ether:ethanol (8:2), dehydrated, filtered, the solvent was evaporated, and the residue was dissolved in methanol 1 ml.
Reference liquid: take l-ephedrine, dissolved in methanol to contain 5 mg of ephedrine control solution.
Expand: Silicone G-plate, developed with n-butanol-glacial acetic acid-water (8:2:1) with a 15 cm spread.
Color development: 0.5% ninhydrin coloring agent, 105 °C baking, for the chromatogram of the test product in the corresponding position with the reference substance showed the same color spots.
Determination of content
Take this product fine powder about 5g, accurately weighed, set Soxhlet extractor, add concentrated ammonia test solution 3ml, ethanol 10ml and ether 20ml, place for 24 hours, add ether on a water bath and heat reflux for 4 hours to alkaloid extract The extract was transferred to a separatory funnel. The container was washed with a small amount of ether. The washing solution was added to a separatory funnel. The solution was shaken with 0.5 mol/L hydrochloric acid solution and extracted 5 times (20 ml, 10 ml, 10 ml, 10 ml, 10 ml). The combined acid solution was filtered, the filtrate was added with a sodium hydroxide solution to make it alkaline, saturated sodium chloride was added, and the solution was extracted 5 times with ethyl ether (20 ml, 10 ml, 10 ml, 10 ml, 10 ml), and the ether solution was combined with chlorine. The sodium saturated solution was washed 3 times, 5 ml each time, and the washings were combined. The solution was then extracted by shaking with ether 10 ml. The secondary ethyl ether solution was combined before and after the addition, and the sulfuric acid titration solution (0.01 mol/L) 30 ml was precisely added and shaken to extract. Place layers. Divide the acid solution; The ether solution is extracted with water 3 times, each time 5ml, and the acid and water are combined. Heat on the water bath to remove trace amounts of ether. Let cool and add 2 drops of methyl red indicator solution. Titrate with sodium hydroxide. Liquid (0.02mol/L) titration. Every 1ml of sulfuric acid titrant (0.01mol/L) is equivalent to 3.305mg of ephedrine (C10H15NO).
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