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The Preparation Of High Purity Lutein And The Synthesis Of Its Derivatives

Posted on:2010-10-12Degree:MasterType:Thesis
Country:ChinaCandidate:L Y ShenFull Text:PDF
GTID:2121360275980359Subject:Chemical processes
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Lutein is a natural pigment,whith have good anti-oxidation performance,increasing people's favor,But in the domestic preparation of high purity lutein is still a vacancy, the major research topics was high-purity lutein preparation,the synthesis of oleic acid lutein and lutein,oleic acid luteind antioxidant research.Marigold include lutein natural is raw materials,is well suited as a raw material for extraction of lutein,the author did research of marigold particle againsting temperature, light,acid,alkaline in order to providing basis for the stockpile of particles marigold.We used cavitation,thermal effects,mechanical action of ultrasonic to speed up the broken of cell wall to the dissolution of lutein in order to improve content,shorten the extraction time.used STATISTICA6.0 software,based on central composite rotatable design(CCRD),we visited impaction of extraction time,extraction temperature,ratio of material to extraction rate.From the response surface we obtained the most excellent conditions of ultrasonic extraction of lutein:extraction temperature:30℃,extraction time:50min,liquid ratio:1:4.Lutein is the main form of ester derivatives in the plant,it has to go through saponification treatment,and will be reverted to the monomer form of lutein.In this study,we speeded up the saponification time,lowered temperature saponification by ultrasonic 'cavitation' and mechanical action to.Using thin-layer chromatography,we inspected the effects of saponification time,saponification temperature,increasing the volume of alkali and the order of increasing alkali saponification to derive optimum saponification conditions:the volume of alkali(10%KOH-methanol solution) was 24 ml,0-60 minutes adding 0.67ml per minute,60-150 minutes adding 0.8ml per 5 minutes,150-190 minutes adding 0.9 ml per 10minute,190-210 minutes adding 0 ml, Ultrasound temperature:40℃,Ultrasonic Time:120 minutes.We studied the separation and purification of lutein by re-crystallization the use of extract(g):tetrahydrofuran(ml):ethanol(ml):petroleum ether(ml):water(ml) =1:20:15:5:20 mixed solvents made the first recrystallization.Acetone,petroleum ether and water mixed solvent make the second re-crystallization.Followed by a four-crystalhigh purity lutein(88%)were made from the low purity of lutein(40%).This study provided an effective means for high-grade of luteinBy direct esterification method,we synthesised oleic acid lutein esters,whith enhanced the stability of lutein out of the body,divided into lutein and oleic acid in the body,met people's demand for lutein and oleic acid.NMR1H,NMR13C,MS,IR analysis showed that the synthesis is success,the author also studied of synthesis of glycine lutein,but in the process of deamination agent,lutein occurred isomerization because of high-temperature environment and the experiment failed.The antioxidant properties of two-oleic acid ester lutein,lutein,lutein oleic acid ester were evaluated by several methods:scavenging effect on hydroxyl,DPPH radical and comparied with antioxidant BHT.The results showed that two-oleic acid ester lutein,lutein,lutein oleic acid ester had the ability of clearing DPPH free radicals, hydroxyl radicals,the sequence of their ability was BHT>lutein>lutein oleic acid monoester>lutein two-oleic acid ester.The conclusions demonstrated that the feasibility of the carotenoid antioxidant connected with the number of conjugated double bonds.The more of number of hydroxyl,the stronger of its antioxidant properties.
Keywords/Search Tags:lutein, preparation, synthesis, oleic acid, response surface, anti-oxidation
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