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Studies On Green Separation Technology Of Eicosahexaenoic Acid Ethyl Ester And Docosahexaenoic Acid Ethyl Ester In Fish Oil

Posted on:2013-10-30Degree:MasterType:Thesis
Country:ChinaCandidate:J J WangFull Text:PDF
GTID:2321330518989147Subject:Drug Analysis
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As a health product,deep sea fish oil has been widely favored,to the human body,its function mainly reflects in the brain intelligence and bright eyes,the prevention and treatment of disease of heart-head-blood-vessel,anti-inflammatory,antitumor,inhibit allergic reaction,etc.Eicopentaenoic acid(EPA)and docosahexenoic acid(DHA)as two main function factor are also be known.To the human body,EPA's function mainly reflects in the prevention and treatment of disease of heart-head-blood-vessel,and DHA's function mainly embodied in the brain intelligence.These two mainly factor reflect different emphasis on the human physiological function,but at present,all the health products from fish oil contain both EPA and DHA.So set up a green technology to separate and purification EPA and DHA from fish oil,producing more selctive fish oil products is very necessary.ObjectiveThis project aims to establish a green technology to separate eicosapentaenoic acid ethyl ester(EPA-EE)and docosahexenoic acid ethyl ester(DHA-EE)from fish oil.And the quick analysis detection method of detecte EPA-EE and DHA-EE in fish oil and its products is studied,as to monitoring the products and the production technology.Methods1?A set of gas chromatography method has been established,to detecte the content of EPA-EE and DHA-EE in the raw material(fish oil)and its products.Constant colum temperature was 240 ?,hold for 15 min,the carrier gas flow velocity was 30 cm/sec,hydrogen velocity was 50 mL/min,air velocity was 400 mL/min,inject temperature was 250?,detector temperature was 250 ?,diversion ratio was 10:1 inI ? L of sample.2?Each single factor of urea inclusion has been studied,the optimal condition of ures inclusion inrich EPA-EE and DHA-EE from fish oil has been determined.Mixed fish oil and urea by 1:3 ratio,reaction 0.5 h in saturated solution of the urea ethanol at 55 ?,then natural cooling to the room temperature,transfer to 0?,keeping 9 h.3?Every single factor of molecular distillation(MD)has been studied,the each optimum molecular distillation condition of distil EPA-EE and DHA-EE from fish oil was selected through orthogonal experiment,and then twice distilled.Best separation conditions of EPA-EE:evaporation temperature 80 ?,condensing temperature 15 ?,saraper speed 100 r/min,pressure 5 Pa.Best separation conditions of DHA-EE:evaporation temperature 90 ?,condensing temperature 20 ?,saraper speed 50 r/min,pressure 5 Pa.Results1?Take 1 ? L fish oil ethyl ester,EPA-EE substance and DHA-EE substance solutions,respectively,detecte by GC.Finally,EPA-EE's retention time in the 6.006 min,DHA-EE's retention time in the 8.896 min,and with the other components to peak baseline separation,meet the analysis detection requirements.2?Through the studied of each single factor of urea inclusion,such as the mixing ratio of fish oil and urea,the reaction time,the reaction temperature,the temperature of urea inclusion,the time of urea inclusion,ect.The auther found that the reaction temperature is the most important factor of the urea inclusion,the mixing ratio of urea and fish oil and the urea inclusion time affect more EPA-EE than DHA-EE in the enrichment product of urea inclusion.The content of EPA-EE and DHA-EE was increased from 17.0%and 13.4%to 54.2%and 21.3%,respectively.The total content of EPA-EE and DHA-EE was increased from 30.4%to 75.5%.3?Each single factor of MD has been studied,such as temperature of heating and degassing in advance,evaporation temperature,condensing temperature,scraper speed,pressure,flow speed,ect.And the results showed that the evaporation temperature is the most important factor to the MD distil EPA-EE and DHA-EE from fish oil,the ccraper speed and the pressure make big effect in the distribution of product in light and heavy.After twice distilled by each optimum conditions,the content of EPA-EE and DHA-EE in product increased from 36.2%and 24.6%to 51.8%and 73.25%,respectively.Conclusions1?This experiment established a GC method which can detecte the content of EPA-EE and DHA-EE in fish oil and its products quickly,and also accurate quantitative,solvent consumption,high sensitivity,good repeatability.2?Enrichment EPA-EE and DHA-EE by urea inclusion low cost,simple operation and easy to industrial production.But urea inclusion cannot separation EPA-EE and DHA-EE from fish oil denpendently,therefore can only as a kind of coarse extraction or pretreatment method,if combine with other method,also can we separated higher purity EPA-EE and DHA-EE.3?MD is by using the mean free path of molecular movement to achieve the purpose of separation and purification.And the whole separation process was in high vacuum condition,and no organic solvent was included.So it can be regarded as a kind of ideal green separation technology.However,as the same sa urea inclusion,MD also can not separate EPA-EE and DHA-EE from fish oil by own,need to combine with other method to get high purity EPA-EE and DHA-EE.
Keywords/Search Tags:fish oil ethyl ester, eicosapentaenoic acid ethyl ester, docosahexaenoic acid ethyl ester, urea inclusion, molecular distillation, superctitical fluid chromatography
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