Method for extracting peganum harmala alkaloid under microwave assistance
A microwave-assisted, camel-spotted technology, applied in the field of microwave-assisted extraction of camel-spotted alkaloids, can solve the problems of large amount of organic reagents, complicated extraction process, and low extraction rate, and achieve automation, short extraction time, and high extraction efficiency Effect
Active Publication Date: 2015-05-20
LANZHOU INST OF ANIMAL SCI & VETERINARY PHARMA OF CAAS
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Problems solved by technology
[0013] The above methods also all have weak points when advancing the camel bald alkaloid extraction technology: 1) although the process is simple when extracting the camel bald alkaloid, the extraction rate is not high
When separating the alkaloid monomers of Camelina alkaloids, chromatographic separation methods such as silica gel columns and macroporous adsorption resins were used. Although 10 compounds were separated, the operation was complicated and was not integrated with modern chromatographic separation techniques; 2) Organic reagents such as chloroform The use of cation exchange resin pollutes the environment, and its regeneration and processing are complicated; 3) although the recovery rate of total alkaloids in the extract is 6.93%, the recovery rate is higher
But when measured by the weight of camel cape seeds, the recovery rate is very low
And the extraction process uses toxic solvents such as chloroform; 4) The extraction process uses heavy metals, which affects the quality of the total alkaloids; 5) The extraction process is complicated, and the amount of organic reagents is large, which increases the cost; 6) After using carbon dioxide critical extraction degreasing, the extraction cost increase, and it is not suitable to filter after acidic ethanol extraction; 7) use organic solvents such as chloroform, which will pollute the environment; 8) the extraction rate of total alkaloids is low, only 40.1mg / g
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Embodiment 1
[0037]Take 1.2g of Camelina seeds, place them in microwave extraction tubes respectively, add ethanol solution with a concentration of 80vt% according to the liquid-to-solid ratio of 30:1 (ml / g), and microwave heating-assisted extraction for 10 minutes at a temperature of 80°C . After cooling, the extract was filtered and analyzed by HPLC. The contents of visicine, harmaline and harmine were 5.859mg / g seed, 38.708mg / g seed and 17.325mg / g seed. The extract was concentrated until there was no alcohol smell to obtain a concentrated solution, which was prepared by chromatographic separation.
[0038] Put the concentrated solution on the preparative high performance liquid chromatography C 18 For a reverse-phase silica gel column, use 0.1mol / L ammonium acetate buffered saline solution (B) with a volume ratio of 70:30 to 96:4. Preparation method: Dissolve 3.4g of ammonium acetate in an appropriate amount of water, then add 3mL of glacial acetic acid solution, and add water to 500m...
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The invention discloses a method for extracting peganum harmala alkaloid under microwave assistance. The method comprises the following steps: drying a peganum harmala plant to a constant weight, using ethanol with volume concentration of 60-95% as a solvent, extracting for 8-12 minutes under microwave heating assistance at a solid-liquid ratio of 10-50 ml / g and an extracting temperature of 60-100 DEG C, filtering to obtain an extracting solution, concentrating the extracting solution until no alcohol smell exists, coating the extracting solution on a preparative high performance liquid chromatography C18 reverse phase silica gel column, using 0.1 mol / L of ammonium acetate buffer salt solution and acetonitrile with a volume ratio of 70:30 to 96:4 as an elution phase, separating and preparing at a flow speed of 1.0 mL / min and within a temperature range of 20-40 DEG C, online monitoring via ultraviolet 280 nm, collecting eluant with a specific absorption peak, and volatilizing to obtain the following three alkaloids: vasicine, banisterine and harmine. The method is simple, convenient, feasible and controllable, and the yield of the alkaloid of the method is higher than that of the existing extraction methods.
Description
technical field [0001] The invention belongs to the technical field of medicines, and in particular relates to a microwave-assisted method for extracting camel alkaloids. Background technique [0002] Peganum harmala (Peganum harmala L.) is a plant of the genus Peganum in the family Zygophyllaceae. The whole plant and seeds are used as medicine, and it is widely distributed in Asia, North Africa and other places. In our country, camel cape mainly grows in the northwest and other places, and is often used as traditional Chinese medicine, Uighur medicine and Mongolian medicinal materials. It has the functions of reducing swelling, relieving pain, dredging blood and regulating menstruation, and is used for joint bone pain, menstrual obstruction, cough and asthma embolism. At present, the compound Luotuoleng ointment with camel's seed as the main ingredient has been put into the market and applied. It has the functions of clearing and purging local abnormal black gallbladder an...
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Login to View More IPC IPC(8): C07D487/04C07D471/04
CPCC07D471/04C07D487/04
Inventor 尚小飞潘虎苗小楼王东升王学智王瑜张继瑜
Owner LANZHOU INST OF ANIMAL SCI & VETERINARY PHARMA OF CAAS
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