Structural Lipid Synthesis And Supercritical Fluid Chromatography Analysis

Medium and long chain triglycerides?MLCT?are very important structural lipids?SLS?and a hot research field in the synthesis of structural lipids.In this study,perilla oil,caprylic acid and capric acid were used as raw materials to prepare MLCT bychemical and lipase catalysis.1.The composition and content of fatty acids in 7 kinds of vegetable oils were analyzed by gas chromatography based on 37 kinds of fatty acid methyl esters analysis.Perilla oil rich in?-linolenic acid?which was long carbon chain polyunsaturated fatty acid?and the medium carbon chain saturated fatty acid?octanoic acid and decanoic acid?were selected as the raw material to prepare MLCT in the form of acidolysis.The standard curves of high purity methyl caproate,methyl decanoate and other fatty acid methyl esters were established in order to determine the content of octanoic acid and decanoic acid in triglycerides and calculate their insertion rate,2.The synthesis of MLCT with perilla oil,caprylic acid and capric acid catalyzed by solid superacid SO4^2-/ZrO₂ was studied.The effects of temperature,time,super acid dosage,fatty acid content and the molar ratio of fatty acid to vegetable oil were studied by single factor experiment.The orthogonal experiment results which based on the single factor experiment showed that the order of influencing factors was as follows:oil/acid molar ratio>reaction time>catalyst dosage>reaction temperature.The optimal reaction conditions were oil/acid molar ratio 1:3,the catalyst amount 3%based on the reactant employed in the reacting system,reacting.at140 o C for 4 h.Under the above experimental conditions,the average insertion rates of caprylic acid and decanoic acid were 3.54%and 7.51%,respectively.The reaction efficiency of chemical synthesis of structured lipids is low.3.Lipase lipozyme TL IM with sn-1,3 site specificity was used as catalyzer to synthesize MLCT structured lipids in the form of acidolysis with perilla oil,octanoic acid and decanoic acid in ionic liquid and supercritical CO₂ systems,respectively.?1?this study focused on synthesizing medium and long chain triglycerides in pure ionic liquid system with perilla oil,octanoic acid and decanoic acid as raw materials and the lipase TL IM.as the catalyst The effects of temperature,time,lipase dosage,fatty acid content and the molar ratio of fatty acid to vegetable oil were studied by single factor experiment.The orthogonal experiment results which based on the single factor experiment showed that the order of influencing factors was as follows:catalyst dosage>oil/acid molar ratio>reaction temperature>reaction time.The optimal reaction conditions were oil/acid molar ratio 1:3,the catalyst amount8%based on the reactant employed in the reacting system,reacting.at 40 ^o C for 15 h.Under the above experimental conditions,the average insertion rates of caprylic acid and decanoic acid were 30.88%and 65.31%,respectively.The reaction efficiency of lipase synthesis of structured lipids is high?2?This study focused on synthesizing medium and long chain triglycerides in supercritical carbon dioxide system with perilla oil,octanoic acid and decanoic acid as raw materials and the lipase TL IM.as the catalyst.The effects of temperature,time,lipase dosage,fatty acid content and the molar ratio of fatty acid to vegetable oil were studied by single factor experiment.The orthogonal experiment results which based on the single factor experiment showed that the order of influencing factors was as follows:reaction time>catalyst dosage>reaction temperature>oil/acid molar ratio.The optimal reaction conditions were oil/acid molar ratio 1:3,the catalyst amount11%based on the reactant employed in the reacting system,reacting.at 40 ^oC for 6 h.Under the above experimental conditions,the average insertion rates of caprylic acid and decanoic acid were 33.16%and 75.30%,respectively.The reaction efficiency of lipase synthesis of structured lipids is high?3?Under the optimal enzymatic synthesis conditions of MLCT in supercritical CO2 system,the preliminary experimental study on the double green mixed system of supercritical CO2 and ionic liquid was carried out.The average insertion rate of caproic acid and decanoic acid were 44.27%and 101 46%,repectivly.The results showed that the mixed system had higher synthesis effciency.4.The effect of catalyzed synthesis of MLCT structured lipids by Lipozyme TL IM in green solvent ionic liquid and supercritical CO2 system was better than solid superacid SO₄^2-/ZrO₂,and the color of product is better.Enzymatic method in supercritical CO₂ system which is a very promising route and system for MLCT synthesis is better than ionic liquid system,5.Supercritical fluid chromatography?SFC?was used to analyze the triglycerides composition of MLCT structured lipid.The types of SFC column,system back pressure,mobile phase B,flow rate and gradient elution procedure were investigated.It was found that the type of chromatographic column and the system back pressure had great influence on the separation effect.The separation effect of the triglycerides composition of MLCT structured lipid was better compared with perilla oil.The ionic fragments of MS was obtained by QDa mass spectrometry.Combined with the carbon number rule,the triglycerides composition types of MLCT structured lipids synthesized were preliminarily deduced based on GC analysis.