Method for preparing sinomenine hydrochloride by using non-organic solvent
A non-organic technology of sinomenine hydrochloride, which is applied in the field of preparation of sinomenine hydrochloride, can solve the problem of high carcinogenesis rate, and achieve the effects of high purity, environmental protection, and no solvent residue
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experiment example 1
[0018] Experimental example 1: Study on the extraction process of Qingfengteng non-organic solvent
[0019] 1. Experimental method
[0020] 1.1 Materials and Instruments
[0021] Qingfengteng crude powder, macroporous adsorption resin, sinomenine hydrochloride reference substance, hydrochloric acid, ammonia water, sodium hydroxide, ethanol, sodium chloride, etc.
[0022] Glass column (diameter 3cm, height 30-40cm), HPLC high-performance liquid phase detector, rotary evaporator.
[0023] 1.2 Methods and results
[0024] 1.2.1 Judgment method
[0025] (1) Selection of alkaloid indicator
[0026] Prepare three alkaloid indicators, bismuth potassium iodide dilute solution, alkaline potassium ferricyanide, and silicotungstic acid test solution, according to the method in Part One of the Chinese Pharmacopoeia 2010 edition, and take 1 to 2 drops respectively in the test solution for precipitation, The color reaction, compared with previous experiments, shows that the indication ...
Embodiment 1
[0084] Embodiment one: a kind of preparation method of the sinomenine hydrochloride of non-organic solvent, this method comprises the steps:
[0085] A. Extraction: 500kg of Qingfengteng coarse powder, wet with 500L of 0.5mol / L HCl for 3 hours, install the percolation cylinder, add 0.5mol / L HCl to make the liquid surface cover the powder by 2cm, soak for 12 hours, press Start percolation at a speed of 3ml / min, stop percolation after 12 hours, obtain percolation liquid, and set aside;
[0086] B. Column elution: Put the treated cation exchange resin or 152 type resin on the percolation liquid, the ratio of diameter to height is 1:10, and the sample loading speed is 3 times the column volume / hour, until the effluent is tested with silicotungstic acid If there is precipitation in the liquid inspection, stop loading the sample when there is no alkaloid spot detected by thin-layer chromatography, and stop when the eluent is eluted with purified water until the eluent has no color, ...
Embodiment 2
[0088] Embodiment two: a kind of preparation method of the sinomenine hydrochloride of non-organic solvent, this method comprises the steps:
[0089] A. Extraction: 800kg of Qingfengteng coarse powder, wet it with 1000L of 0.9mol / L HCl for 5 hours, install the percolation cylinder, add 0.9mol / L HCl to make the liquid surface cover the powder by 2cm, after soaking for 20 hours, press Start percolation at a speed of 5ml / min, stop percolation after 24 hours, obtain percolation liquid, and set aside;
[0090] B. Column elution: put the treated cation exchange resin 001*4 type or 152 type resin on the percolation liquid, the ratio of diameter to height is 1:10, and the loading speed is 5 times the column volume / hour, until the effluent is used If there is precipitation in the silicotungstic acid test solution, stop loading the sample when there is no alkaloid spot detected by thin-layer chromatography, and stop when the eluent is colorless by elution with purified water, soak the r...
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