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Dołączył: 26 Paź 2010
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| Temat postu: scarpe mbt Hong shoot spider Extraction and analys |
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Hong shoot spider Extraction and analysis of volatile components
, And after testing found a simple, low cost,[link widoczny dla zalogowanych], can generate the scale of the extraction, synthesis process. An instrument and reagent ZX98 ~ 1 rotary evaporator (Shanghai Institute of Organic Chemistry); 81-2 type constant temperature magnetic stirrer (Shanghai Music Instrument Division); WS70-1 Fast Infrared dryer. Artemisia annua (Chongqing Institute of Chinese Medicine); silica gel plates and silica gel (100 ~ 200 300 ~ 400 mesh, Yantai City, Zhi Gang Huang service development pilot plant silica); other chemical reagents (commercially available, chemical pure). 2 Methods and Results 2,1 artemisinin extraction methods: the broken rear 50g dried Artemisia annua 250mL conical flask, followed by soaking with 200,150,100 mL petroleum ether, 24h, filtration, combined filtrate after 35 4O ℃ in vacuum concentrated, crude artemisinin too oily. Purification of artemisinin: Weigh 300 to 400 mesh silica gel column packing 16.003g, artemisinin dissolved in the crude methylene chloride on a wet column, with 200mL of a petroleum ether eluant 【ethyl acetate (10:1 ) To make a quick column chromatography. By thin layer chromatography (TLC) examination of a 【petroleum ether acetone (4:1) as the agent】 collection combined active ingredients, concentration, after standing at least the amount of volume crystallization. Filtration,[link widoczny dla zalogowanych], cake washing a small amount of petroleum ether, to white, drying pure Artemisinin 64mg, yield 0.13%, the melting point of 151 ~ 152.5oC. Synthesis of Artemether: 60mg of artemisinin will be dissolved in 2mL of pure methanol, add to the 10mL eggplant-shaped flask, add batches under ice bath cooling 53.116mgNaBH, heat reaction 1.5h, to the TLC test 【 ],[Put it aside for crystallization, absorb liquor, add 2mL saturated salt water, filtration, repeated washing with 1mL distilled water after drying the filter cake three times,[link widoczny dla zalogowanych], re-crystallization of artemether 48mg, yield 75.8%, the melting point of 85. 2 ~ 87.0oC. Synthetic route shown in Figure 1. Figure 1 The synthetic route of artemether 2.2 Results of the synthesis and purification of artemisinin and artemether reduced the melting point of synthesis, the reaction occurs more easily, thereby increasing the yield. 3 discussion of the method is simple, short,[link widoczny dla zalogowanych], without the use of special reagents and equipment, and other artemisinin extraction and purification methods, from pure artemisinin can be achieved without active carbon and other purity requirements, and eluent concentration after a certain volume to make artemisinin crystals. The synthetic method for the improvement of existing technology to provide a basis for extraction of artemisinin.
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