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Preparation and Characterization of the High Purity of Solanesol

Author: ZhouYongSheng
Tutor: CaiChun;FangYongQin
School: Nanjing University of Technology and Engineering
Course: Applied Chemistry
Keywords: High purity solanesol The supercritical CO2 quadratic static extraction Column chromatography Recrystallization Liquid chromatography - mass spectrometry
CLC: TQ223.1
Type: Master's thesis
Year: 2009
Downloads: 57
Quote: 1
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Abstract


Solanesol as an important pharmaceutical intermediates , synthetic medical coenzyme Q 10 and vitamin K 2 key raw materials . Its longer carbon chain synthesis steps can not be synthesized mainly by tobacco extract . In this paper, supercritical CO 2 static , dynamic , static and dynamic binding and secondary the static four extraction methods solanesol in tobacco leaves crude extract secondary static extraction extract better . By orthogonal experiments investigated the second static extraction temperature , pressure , time and entrainer factors extracted solanesol composite indicator . Optimal conditions : the entrainer 95% ethanol , liquid to solid ratio of 5.0 mL / g , 60 ° C , 45MPa under extraction 1h . This condition solanesol the selective extraction rate and transfer rate of 31.59% , 3.81% and 97.69% , respectively . The experiment also improved Soxhlet extraction method to extract solanesol crude . Ethanol as the extraction solvent , liquid to solid ratio of 30 mL / g refluxed for 4 h at 70 ° C , the solanesol selective extraction rate and transfer rate of 26.03% , 2.84% and 72.82% , followed by . The experiments show that the improved Soxhlet extraction , supercritical CO 2 secondary static extraction has a significant advantage . Petroleum ether - ethyl acetate (4:1, v / v) mixed solution as the eluent, from the content of 31.59% solanesol crude product was purified by column chromatography separation to obtain a content of 85.01% solanesol , and then by recrystallized 98.62% high purity solanesol . Product structures were confirmed by IR , 1 H NMR 13 C NMR and ESI-MS characterization of the target product 3,7,11,15,19,23,27,31 35 - nine methyl -2,6,10,14,18,22,26,30,34 - 9 , hexadecane -1 - match the characteristics of the alcohol . The supercritical CO 2 secondary static extraction of crude extract of tobacco solanesol extraction rate and the transfer rate is higher than the existing method , the easing of the process conditions and environment friendly alternative to traditional heat reflux extraction ; using column chromatography - recrystallization joint prepared containing ≥ 98% high purity solanesol , the total yield of 1.58% , can provide good guidance for the industrial scale .

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CLC: > Industrial Technology > Chemical Industry > Basic Organic Chemistry Industry > The production of aliphatic compounds ( acyclic compounds) > Aliphatic alcohols (alcohols, hydroxy compounds) and its derivatives > Aliphatic alcohol
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