Study On Preparation And Purification Of Conjugated Linoleic Acid Diglycerides

Diglycerides always called DAG for short,produced by glycerol and two fatty acid,is savageness component in edible oils,and the inter-production in metabolize by oils,concluded in GRAS,safety,nutrition,fit for processing,easiness for body and so on virtue,attribute to functional additive,applied for food,cosmetic,and medica,also attribute to single type food class emulsification,and have no difference between edible oils in edible sense,colour,taste.There are few DAG in savageness plants,so it is important to prepare DAG by oils.This paper study on preparation technology of DAG mainly,from Purification of linoleic acid from corn Oil with urea adduction fractionation,prepare CLA material to emphases on prepare DAG by esterification mathod,Purificate production by molecule distillation,discussed influence of centrifugation on purification of linoleic acid from corn oil with urea adduction fractionation,and synthesize DAG by Immobilized lipase Lipozyme TL IM.This article has done below the research and obtains the conclusion:ONE,Saponification and decompose to prepare linoleic mixture by corn oils,Purification high content linoleic with urea adduction fractionation,change structure of linoleic by alkali,the best parameter made certain in this experiment.In this conditions,the temperature is 15℃,centrifugation speed is 3000r/min,centrifugation time is10min,the linoleic content of from fatty acid mixture improved from 55.61%to 66.26%by centrifugation,compared with mixed fatty acids before centrifugation,content of linoleic acid is increased 12.29%,content of linoleic acid achieved 93.99%,in urea adduction fractionation experiment,the best parameter were fatty acid/urea/ethanol is 1:1.5:3,fractionation temperature is 15℃,time is 12 hour more suitable,effect of dissolving urea by different concentration of ethanol from 80%～100%on linoleic acid was researched,the results indicate that:The difference between iodine value and recovery of linoleic acid is not remarkable,so recycle ethanol may used again.As index of efficience of transformation,confirm the best parameter by single factor experiment and orthogonal experiment,get results:reaction temperature 170℃,time 4h,alkali to fatty acid 0.4,solvent to alkali 3 or 4.Validation experiment was done by the best parameter, efficience of transformation is 95%.We get the exact result of conjugated linoleic acid content by GC method,the c9,t11 and t10,c12 structure of conjugated linoleic acid are 40.011%and 42.192%.Scaning the all spectrums of production of preparation by UV and FT-IR,compared with the standards,the analysis results indicated:conjugated linoleic acid is the preparation production.TWO,As the process of producting 1,3-Conjugated linoleic acid Diglycerides,added glycerol adsorbption material can avoid phenomenon of enzyme grouped,convenient for mixing,reaction equality,enzyme can be cycled,the material of glycerol adsorbption more appropriate for AL302,in this condition that:mol ratio of fatty and glycerol is 2:1,content of enzyme added is 15%bottom material,temperature is 70℃,time is 6 h,quality ratio silica gel to glycerol is 1:1,glycerol adsorbption material added may delay using times of enzyme, esterification rate may improve 20%,silca gel added may extend enzyme repeat times;the regressin equation was get by single factor experiment and orthogonal experiment before DPS soft processing.Y=71.38714+2.35701XJ₁+0.70723X₂+0.97932X₃-0.62125X₁X₂-0.64375X₁X₃ -5.12326X₁²-1.39327X₂² -0.62076X₃²The best combination of esterification rate is X₁=0.1827,X₂=0.1023,X₃=0.6554,namely ,the best precept of producting 1,3-Conjugated linoleic acid Diglycerides is:mol ratio of fatty and glycerol is 2.11%,content of enzyme added is 15.30%,weight ratio of glycerol adsorbption material and glycerol is 1.20%,reaction temperature is 70℃,reaction time is 10h,the esterification rate is 71.96%in this condition,acid value of mixture is 58.4,monoglycerol content is 26.4%,diglycerides content is 42.5%,triglycerides content is 9.4%,fatty acid content is 21.7%.Three,Two classes process molecule distillation technology were made use of purifying 1,3-Conjugated linoleic acid diglycerides,confirm the purification technics of molecule distillation:feed temperature is 70～80℃,feed speed is 0.4～0.51./h,first class process temperature is 130℃～140℃,two class process temperature is 210℃～220℃,distillion pressure is 0.1Pa,speed is 280～320 r/min,in this condition the effect is better,after two class process molecule distillation,and separate by TLC,monoglycerol content is 2.4%,diglycerides content is 77.4%,triglycerides content is 17.2%,fatty acid content is 3.0%.