CN102864189B - Method for preparing alpha-linolenic acid based on urea envelope method of molecular distillation - Google Patents
Method for preparing alpha-linolenic acid based on urea envelope method of molecular distillation Download PDFInfo
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Abstract
The invention discloses a method for extracting purified alpha-linolenic acid by combining molecular distillation and a urea envelope method with perilla oil as raw materials and belongs to the technical field of profound processing and comprehensive utilization of fat. The method includes that the perilla oil on the market is used as raw materials, lipase is added for hydrolysis to obtain fatty acid mixture, the fatty acid mixture is initially purified through the molecular distillation technology, further purification is conducted through the urea envelope method, and alpha-linolenic acid products are obtained through operations such as petroleum ether extraction and reduced pressure distillation. In areas of north China, central China, northwest and the like, oil resources rich in polyunsaturated fatty acid are abundant, the method is applied to profound processing of the oil resources, not only good polyunsaturated fatty acid products can be provided, and simultaneously economical additional value of the oil crop is improved.
Description
Technical field
The present invention relates to the grease manufacture field, is specially the method for the standby purifying alpha-linolenic acid of a kind of urea clathrate legal system based on molecular distillation.
Background technology
(one of important plant material of α-LNA) is perillaseed to alpha-linolenic acid.Perillaseed has two types of purple perilla and common perillas, is the highest species of alpha-linolenic acid content in now known plant, and oleaginousness is 45%～50%, and wherein alpha-linolenic acid content is in 60% left and right.Experiment shows, alpha-linolenic acid has different physiological roles.For example: cardioprotection, liver, the prevention cardiovascular and cerebrovascular diseases improves memory, delays senility, and preventing apoplectic strengthens fecundity etc.Therefore the activity research and the application that the extraction purifying research of alpha-linolenic acid be can be alpha-linolenic acid lay the foundation.
Alpha-linolenic acid is the straight chain fatty acid that contains 18 carbon atoms, three two keys, belongs to omega-3 polyunsaturated fatty acids series.Due to the nonsaturation of its height, thereby oxidizing reaction easily occurs under hot conditions; The isomerization reaction of position of double bond and configuration easily occurs under alkaline condition, forms Conjugated polyenoic acids.So in order effectively to protect the physiologically active of alpha-linolenic acid, the selection of preparation alpha-linolenic acid processing condition seems particularly important.The preparation of alpha-linolenic acid comprises two large processes, is at first by the mixed lipid acid of raw oil material hydrolysis preparation, more further extracts purifying and get linolenic acid.In the process of preparation mixed fatty acid, usually adopt the methods such as traditional saponification, acidolysis both at home and abroad, because reaction conditions is violent, oxidation, polymerization, isomerization can occur in polyunsaturated fatty acid, certainly will affect the alpha-linolenic acid functional performance.With the development of enzyme engineering technology, the research of using the enzymatic hydrolysis grease increases gradually, and report is all arranged both at home and abroad.
For the alpha-linolenic acid purification process, mainly contain at present silver ion complexation, column chromatography, freeze crystallization, supercritical extraction method etc., but these methods exist such as dissolvent residual, purity are not high, yield is low, purifying cycle length, environmental pollution, to shortcomings such as equipment requirements height.
Molecular distillation method refers under high vacuum condition, the liquid ingredient liquid level of overflowing at the temperature lower than boiling point.Greater than the weight molecule mean free path, and velocity of evaporation is fast due to the mean free path of light molecule, thereby light molecule in mixture is constantly overflowed and realizes the purpose of weight molecular separation.The characteristics of molecular distillation are that vacuum tightness is high, distillation temperature is short lower than vacuum distilling and the material heated time of routine, are conducive to protect the physiologically active of alpha-linolenic acid, and without organic solvent, environmental pollution is little.Utilize molecular size range to come separation of fatty acids, can the different lipid acid of separation of carbon atom number, but the different lipid acid of the identical saturation ratio of carbonatoms is difficult to separate.And the urea clathrate method is the method for separating according to the molecule saturation ratio.The crystallization of urea is tetragonal body, becomes the hexahedron crystal when coexisting with straight chain fatty acid.Linear saturated fatty acids the most easily enters in the pipeline of hexahedron crystal, and forms the urea clathrate thing.And the two keys in unsaturated fatty acids are more, and in the pipeline of crystal more difficult to get access, two keys increase molecular volume, more difficult formation urea clathrate thing.According to this property, high unsaturated fatty acid and saturated and low unsaturated fatty acids can be separated, reach the purpose of separating alpha-linolenic acid.
The present invention is directed to the structure of alpha-linolenic acid and the testing program that character has designed purifying alpha-linolenic acid, namely adopt biological hydrolysis method (lipase hydrolysis method), and the technology such as binding molecule distillation and urea clathrate method are carried out separating-purifying to alpha-linolenic acid in vegetables oil.At first be to adopt the lipase hydrolysis raw oil material, and the G ﹠ W of fully removing in enzymolysis solution divides, obtain concentrated mixed lipid acid; In further extracting the purifying alpha-linolenic acid process, molecular distillation technique and urea clathrate method have been used.Enzymic hydrolysis, the relative gentle technique of three kinds of conditions of molecular distillation and urea clathrate method combine, and can prevent effectively that two keys of alpha-linolenic acid are not oxidized, thereby protect the functional performance of alpha-linolenic acid; Simultaneously, process by molecular distillation, in mixed fatty acid, a large amount of low-molecular-weight light constituents are separated, in the lipid acid concentrated solution, alpha-linolenic acid content is high, consume less reagent in the urea clathrate test and obtain efficient envelope effect, when making alpha-linolenic acid obtain effective purifying, reduce pollution, reached the purpose of energy-saving and emission-reduction.For the purifying of alpha-linolenic acid, being in the great majority of single employing urea clathrate method or beta-cyclodextrin inclusion compound method adopts the molecular distillation method purifying process to rarely have report, and the especially use of molecular distillation and urea clathrate method combined technology is there are no bibliographical information.
Therefore, providing the method for the standby alpha-linolenic acid of a kind of urea clathrate legal system based on molecular distillation, has been a problem of needing solution badly.
Summary of the invention
In order to overcome above-mentioned deficiency of the prior art, the invention provides the method for the standby alpha-linolenic acid of a kind of urea clathrate legal system based on molecular distillation.by test, the enzyme hydrolysis condition of vegetables oil and the experiment condition of urea clathrate purifying alpha-linolenic acid are optimized, choosing the perilla oil that is rich in alpha-linolenic acid is that raw material prepares alpha-linolenic acid, its basic step is: the selection of raw material, lipase hydrolysis prepares mixed fatty acid, and the G ﹠ W of fully removing in protease hydrolysate divides, molecular distillation method is isolated light phase component with the preliminary purification mixed fatty acid, then use the urea clathrate method to be further purified linolenic acid, especially hydrolysising condition and the urea clathrate condition of lipase have been carried out systematic study, obtain content of the present invention:
The object of the present invention is achieved like this:
The method of the standby purifying alpha-linolenic acid of a kind of urea clathrate legal system based on molecular distillation comprises the following steps:
(1) selection of raw material: choosing the perilla oil that is rich in alpha-linolenic acid is raw material, and commercially available perilla oil directly uses;
(2) lipase hydrolysis prepares the mixed fatty acid enzymolysis solution: the hydrolysising condition of perilla oil is as follows, and (perilla oil: lipase: water) be 25:1:50 (m:m:V), hydrolysis temperature is set to 45 ℃ to the material ratio, hydrolysis time 6 h;
(3) the abundant removal of glycerine and moisture in enzymolysis solution: at first utilize separating funnel to isolate water; Add 30 ℃ of warm water slowly to rock in oil phase rear standing, separating funnel separates for the second time; Under 5000r/min, 0 ℃ of condition centrifugal 5 minutes, remove moisture through rotary evaporation;
(4) molecular distillation method preliminary purification mixed fatty acid: the mixed fatty acid that the upper step was obtained uses the molecular distillation method separation concentrated, and discard light phase component: distillation condition is scraper plate rotating speed 20r/min, 112 ℃ of temperature of heating plate, pressure 8mtorr;
(5) the urea clathrate method is further extracted purifying alpha-linolenic acid: the envelope solvent is methyl alcohol or ethanol; Envelope requirement is that the envelope ratio is 1:6:2,1:8:1,1:8:2,1:8:3 or 1:10:2, and the envelope temperature is-10 ° of C ~ 30 ° C, and the envelope time is 2 ~ 12h;
In the step of urea clathrate method purifying alpha-linolenic acid, the envelope effect of methanol solvate is better than ethanol.
In the step of urea clathrate method purifying alpha-linolenic acid, optimum envelope requirement is: the envelope ratio is 1:8:2, and the envelope temperature is 0 ° of C, and the envelope time is 4h.
To sum up, in the present invention, the scheme of preparation method's optimum is:
Take perilla oil as raw material, (perilla oil: lipase: water) be 25:1:50 (m:m:V), be hydrolyzed 6h at 45 ℃ of temperature, enzymolysis solution must concentrate mixed fatty acid through fully removing after G ﹠ W divides to the material ratio, and its acid value is about 140, yield 78%; Carry out molecular distillation concentrated (one or twice) under the distillation condition of scraper plate rotating speed 20r/min, 112 ℃ of temperature of heating plate, pressure 8mtorr, the mixed fatty acid acid value that obtains is 200 left and right; On the basis of urea clathrate method experiment of single factor, the test of design response surface analysis, data analysis shows that three single factors are little to the reciprocal effect of result, the optimum reaction condition of determining is 0 ℃ of envelope temperature, envelope times 4 h, envelope ratio lipid acid: methyl alcohol: when urea (m:V:m) is 1:8:2.Three proof tests under top condition, the alpha-linolenic acid average content that obtains product are that 82.70%(is that alpha-linolenic acid content brings up to 82.70% by 55.34%), yield is 52.2%.
Beneficial effect:
The first, the mild condition of enzymatic hydrolysis oil plant and molecular distillation method purifying can prevent effectively that two keys of alpha-linolenic acid are not oxidized, thereby has protected the physiologically active of alpha-linolenic acid;
Second, process by molecular distillation, in mixed fatty acid, a large amount of low-molecular-weight light constituents are separated, in the lipid acid concentrated solution of preliminary purification, alpha-linolenic acid content is high, urea clathrate test consumption is few, when making alpha-linolenic acid obtain effective purifying, reduce pollution, reached the purpose of energy-conserving and environment-protective.
The 3rd, be at first the preparation of pure mixed fatty acid in the large step of preparation alpha-linolenic acid two, then carry out the extraction purifying of alpha-linolenic acid.Usually adopt the methods such as traditional saponification, acidolysis to prepare mixed fatty acid both at home and abroad, because reaction conditions is violent, to polyunsaturated fatty acid, oxidation, polymerization, isomerization can occur, certainly will affect the alpha-linolenic acid functional performance; With the development of enzyme engineering technology, the research of using the enzymatic hydrolysis grease increases gradually, and report is all arranged both at home and abroad.For the purifying of alpha-linolenic acid, being in the great majority of single employing urea clathrate method or beta-cyclodextrin inclusion compound method adopts the purifying process of molecular distillation method to rarely have report, and the especially use of molecular distillation and urea clathrate method combined technology is there are no bibliographical information.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated:
Material used in the present invention is: perilla oil (commercial); Lipase (the bright company far away in Guangzhou); Potassium hydroxide solution; Sherwood oil (boiling range 60-90 ℃, Kaifeng chemical reagent head factory); Ethanol (95%, Tianjin good fortune chemical reagent factory in morning); Anhydrous sodium sulphate (Tianjin Kermel Chemical Reagent Co., Ltd.); Urea (analytical pure, Luoyang chemical reagent factory); Boron trifluoride diethyl etherate (Chemical Reagent Co., Ltd., Sinopharm Group); Methyl alcohol (analytical pure, Luoyang City's chemical reagent factory); Normal heptane (Tianjin section close europeanized reagent company limited); Sodium-chlor (analytical pure, Suzhou chemical reagent factory).
The equipment that the present invention uses comprises: water-bath constant temperature oscillator SHA-C(Jintan City magnificent cutting edge of a knife or a sword Instr Ltd.); Cryogenic thermostat reactive bath technique DF-10L/40(Henan intelligence prestige development in science and technology company limited); Rotatory evaporator RE-52A(Shanghai Yarong Biochemical Instrument Plant); Circulating water type vacuum pump SHZ-D (III) (Yuhua Instrument Co., Ltd., Gongyi City); Gas chromatograph 9790(FULI); Hydrogen generator GHL-300(Beijing is converged good); Air generator (Beijing is converged good); Molecular distillation instrument Wiped-Film Hybrid Still System(U.S. POPE company).
The acid value determination method that relates in the present invention adopts GB/T 5530-2005: take approximately 0.423g uniformly mixed lipid acid in Erlenmeyer flask, add ether-ethanol (2:1) mixed solvent 50mL, shake and make its dissolving; Add three phenolphthalein indicators, drop to blush with about 0.1mol/L potassium hydroxide solution, and 30 seconds colour-fast, write down the potassium hydroxide solution volume V(mL of consumption).
In acid value (mgKOH/g oil)=V * c * 56.1/m formula, V (mL) is the volume of potassium hydroxide standardized solution used; C (mol/L) is the accurate concentration of potassium hydroxide standardized solution used; M (g) is the quality of sample; 56.1 (g/mol) be the molar mass of potassium hydroxide.
Involved in the present invention to the distillation condition that adopts of molecular distillation method preliminary purification alpha-linolenic acid be: scraper plate rotating speed 20r/min; 112 ℃ of temperature of heating plate; Pressure 8mtorr.Begin charging after the instrument normal operation, the speed of charging is difficult for too fast, otherwise can separate not exclusively.Discard light phase component after having separated, if separate not exclusively operate for the second time.
Involved in the present invention to the envelope test method be: accurately take the mixed fatty acid after enzymolysis, add successively lipid acid, methyl alcohol or ethanol (95%), urea in different envelope ratios, temperature is 75 ℃ of lower reflux and constantly vibrates to the transparent clarification of solution, so that urea dissolves and evenly fully mixes with lipid acid and solvent; After being cooled to room temperature, select differing temps and time to carry out the envelope reaction; Taking-up after the envelope reaction is completed, rapid suction filtration, liquid phase is for being rich in linolenic mixed fatty acid.For washing away a small amount of urea of sneaking into, add little water in liquid phase after, use the two volumes petroleum ether extraction; Repeat to wash 2-3 time, collect petroleum ether layer, in 35 ℃ of lower underpressure distillation desolventizings (recycling), obtain mixed fatty acid, weigh and calculated yield (yield is the quality of the front mixed lipid acid of quality/urea clathrate of mixed lipid acid after urea clathrate).
Gas chromatographic analysis operating process involved in the present invention is: get about 350 mg oil samples and put into 50 mL flasks, add 7 mL boron trifluoride methanol solution, add a zeolite reflux 2 minutes, and added 3.5 mL normal heptanes to reflux again one minute from the prolong upper end.Withdraw burning things which may cause a fire disaster, take out flask, add a certain amount of sodium chloride saturated solution in flask, after turning upside down gently for several times, standing demix.Take out approximately 2mL solution upper strata liquid in flask and transfer in rub oral examination tube, add appropriate anhydrous sodium sulphate to remove micro-moisture, obtain the esterification sample in order to gas chromatographic analysis.GC conditions is: sample size: 0.2 μ L; Post case temperature: 190 ℃; Adopt FID(hydrogen ion flame) detector, detected temperatures: 250 ℃; Auxiliary I temperature: 250 ℃; Carrier gas nitrogen pressure 0.5MPa; Hydrogen pressure is 0.1MPa; Air pressure is 0.13MPa.
Realization of the present invention comprises the following steps:
Step 1 raw material is processed
Commercially available perilla oil directly uses.
Step 2 lipase hydrolysis prepares mixed fatty acid
Get the perilla oil of 100g, 4g lipase, 200 mL water are in 500 mL tool plug Erlenmeyer flasks.Put into water-bath constant temperature oscillator after sealing, temperature setting is set to 45 ℃.Take out after 6 h, separating funnel isolated for disposal water, add 30 ℃ of warm water slowly to rock in oil phase rear standing, separating funnel is isolated water for the second time, oil phase under 5000r/min, 0 ℃ of condition centrifugal 5 minutes, the concentrated mixed fatty acid that removes moisture through rotary evaporation adopts GB/T 5530-2005 to measure acid value.
The enzymic hydrolysis temperature is 45 ℃, wherein the m(perilla oil): m(lipase): V(H
2O) be 25:1:50, the mixed fatty acid acid value for preparing is about 140, yield 78%.
Step 3 molecular distillation method preliminary purification mixed fatty acid
Distillation condition: scraper plate rotating speed 20r/min; 112 ℃ of temperature of heating plate; Pressure 8mtorr.Begin charging after the instrument normal operation, the speed of charging is difficult for too fast otherwise can separates not exclusively.Separated the light phase product of rear collection.After adopting molecular distillation concentrated, the mixed fatty acid acid value that obtains is 200 left and right; This step gets mixed fatty acid through gas chromatographic analysis, and the content of its alpha-linolenic acid is approximately 55.34%, and its gas-chromatography appearance time is 19 min; Linoleic content is 10.6%, and oleic acid content is 19.3%, and palmitic acid content is 9.7%.
Step 4 urea clathrate method purifying
The selection of envelope solvent
According to the bibliography contrived experiment: temperature is-6 ℃, lipid acid: methyl alcohol or ethanol (95%): urea (m/V/m) is that 1:8:2(is hereinafter to be referred as the envelope ratio).Experimental design such as table 1:
Table
The experimental design condition
| Group | Solvent | The envelope ratio | Time (h) | Temperature (℃) |
| 1 | Methyl alcohol | 1:8:2 | 12 | -6 |
| 2 | Ethanol | 1:8:2 | 12 | -6 |
The product that obtains is through the laggard promoting the circulation of qi analysis of hplc of esterification, and table 2 is that methyl alcohol and alcohol solvent are on the impact of envelope product yield and linolenic acid content.
Table 2 envelope solvent affects result to experiment
| Group | Solvent | Lipid acid quality (g) | Yield | Content |
| 1 | Methyl alcohol | 4.40 | 44.0% | 84.8% |
| 2 | Ethanol | 3.20 | 32.0% | 81.8% |
As can be seen from Table 2, be that yield or alpha-linolenic acid content are all than the height with alcohol solvent no matter methyl alcohol is made solvent.As seen, use the effect of methanol solvate to be better than ethanol, this conforms to bibliographical information, so following test and Selection anhydrous methanol is the envelope solvent.
For uric acid envelope reaction, envelope time, envelope temperature, envelope ratio are the principal elements that affects the envelope effect, so this experiment is optimized these factors, to finding best envelope requirement.
The envelope time
Constant envelope temperature (10 ℃), lipid acid: methyl alcohol: urea=1:8:2, experimental design is as shown in table 3.
Table 3 experimental design condition
| Group | The envelope time (h) | The envelope ratio | Temperature (℃) |
| 1 | 2 | 1:8:2 | -10 |
| 2 | 4 | 1:8:2 | -10 |
| 3 | 6 | 1:8:2 | -10 |
| 4 | 8 | 1:8:2 | -10 |
| 5 | 12 | 1:8:2 | -10 |
The envelope product is through gas chromatographic analysis, and the yield of each set product linolenic acid content and correspondence is as shown in table 4.
The impact of table 4 envelope time on experimental result
| Group | The envelope time (h) | Mixed fatty acid quality (g) | Yield | Content |
| 1 | 2 | 4.96 | 49.6% | 85.8% |
| 2 | 4 | 4.46 | 44.6% | 86.2% |
| 3 | 6 | 4.23 | 42.3% | 86.2% |
| 4 | 8 | 3.63 | 36.3% | 83.9% |
| 5 | 12 | 3.13 | 31.3% | 85.0% |
* constant envelope temperature-10 ℃, envelope ratio 1:8:2
As can be seen from Table 4, when being 4 h and 6 h, the content of alpha-linolenic acid reaches maximum value the envelope time.When the network time was 4 h, the content of alpha-linolenic acid was very high and yield is also higher, descended over alpha-linolenic acid yield after 4 h a lot.Relatively comprehensive, think that envelope times 4 h is relatively good, its alpha-linolenic acid content is 86.2%, yield is 44.6%.
The envelope temperature
Taking mixed fatty acid 10 g, in 1:8:2(m:V:m) ratio adds lipid acid, methyl alcohol, urea successively.Temperature is 75 ℃ of lower reflux and constantly vibrates to the transparent clarification of solution.After cooling under room temperature, at differing temps lower envelope 4 h.Experimental design is as shown in table 5::
Table 5 experimental design condition
| Group | Temperature (℃) | The envelope ratio | Time (h) |
| 1 | 30 | 1:8:2 | 4 |
| 2 | 20 | 1:8:2 | 4 |
| 3 | 10 | 1:8:2 | 4 |
| 4 | 0 | 1:8:2 | 4 |
| 5 | -10 | 1:8:2 | 4 |
Through gas chromatographic analysis, the yield of the linolenic acid content of envelope product and correspondence is as shown in table 6.
The impact of table 6 envelope temperature on experimental result
| Group | Temperature (℃) | Lipid acid quality (g) | Yield | Content |
| 1 | 30 | 6.18 | 61.8% | 73.3% |
| 2 | 20 | 4.36 | 43.6% | 78.9% |
| 3 | 10 | 4.80 | 48.0% | 80.9% |
| 4 | 0 | 4.96 | 49.6% | 80.6% |
| 5 | -10 | 3.20 | 32.0% | 81.1% |
* constant envelope times 4 h, envelope ratio 1:8:2
As seen from Table 6: with the reduction of temperature, alpha-linolenic acid content increases.When being in 10 ℃, 0 ℃ ,-10 ℃, the content of alpha-linolenic acid remains unchanged substantially.The yield of alpha-linolenic acid descends more when temperature is-10 ℃.When Tc was low, the content of alpha-linolenic acid was higher, and this is because the formation of urea clathrate thing is the process of a heat release, and when temperature descended, reaction was carried out to the direction that generates the urea clathrate thing.In the time of 0 ℃, the yield of alpha-linolenic acid is the highest, comprehensively relatively selects Tc to be 0 ℃ and is more excellent temperature.
The envelope ratio
Constant envelope temperature-6 ℃, envelope times 12 h is in different envelope ratios such as table 7 contrived experiment.
Table 7 experimental design condition
| Group | The envelope ratio | Time (h) | Temperature (℃) |
| 1 | 1:10:2 | 12 | -6 |
| 2 | 1:8:1 | 12 | -6 |
| 3 | 1:8:2 | 12 | -6 |
| 4 | 1:8:3 | 12 | -6 |
| 5 | 1:6:2 | 12 | -6 |
Through gas chromatographic analysis, the yield of the linolenic acid content of envelope product and correspondence is as shown in table 8.
The impact of table 8 envelope ratio on experimental result
| Group | The envelope ratio | Mixed fatty acid quality (g) | Yield | Content |
| 1 | 1:10:2 | 3.64 | 36.4％ | 82.6％ |
| 2 | 1:8:1 | 7.38 | 73.8% | 70.8% |
| 3 | 1:8:2 | 3.65 | 36.5% | 83.9% |
| 4 | 1:8:3 | 3.45 | 34.5% | 87.2% |
| 5 | 1:6:2 | 3.08 | 30.8% | 85.2% |
* constant envelope times 12 h, envelope temperature-6 ℃
By table 8, relatively test as can be known for the the 1st, the 3rd, the 5th group, along with the increase of methanol usage, the content of alpha-linolenic acid is very little, and this is because the consumption of urea is a remarkable factor that affects alpha-linolenic acid content.Can find out from experimental result: in different its liquid phases of envelope ratio, the content of alpha-linolenic acid and yield are all not identical yet.Take into account both, we think that the 3rd group is lipid acid: methyl alcohol: urea=1:8:2 is selection preferably, and wherein alpha-linolenic acid content is 83.9%, and yield is 36.5%.
On the basis of single factor experiment, take the content of alpha-linolenic acid and yield as index, selecting envelope temperature (10,0,10 ℃), envelope time (2,4,6h) and envelope ratio (1:8:1,1:8:2,1:8:3) is factor, tests according to 20 groups of response surfaces of response surface software design.According to the response surface analysis result, determine that 0 ℃ of envelope temperature, envelope times 4 h, envelope ratio are that 1:8:2 is best envelope reaction conditions.Carry out with this understanding confirmatory experiment three times, the average content that obtains alpha-linolenic acid is 82.7%, and average yield is 52.2%.
Above embodiment only is used for explanation the preferred embodiment of the present invention; but the present invention is not limited to above-mentioned embodiment; in the ken that described field those of ordinary skill possesses; it any modification of doing within the spirit and principles in the present invention, is equal to and substitutes and improvement etc., within all should be encompassed in the technical scheme scope that the present invention asks for protection.
Claims (1)
1. method based on the standby purifying alpha-linolenic acid of the urea clathrate legal system of molecular distillation comprises the following steps:
(1) selection of raw material: raw material is the perilla oil that is rich in alpha-linolenic acid;
(2) lipase hydrolysis prepares the mixed fatty acid enzymolysis solution: the hydrolysising condition of perilla oil is as follows, and the material ratio is perilla oil: lipase: water=25:1:50, hydrolysis temperature are set to 45 ℃, hydrolysis time 6 h;
(3) the abundant removal of glycerine and moisture in enzymolysis solution: at first utilize separating funnel to isolate water; Add 30 ℃ of warm water slowly to rock in oil phase rear standing, separating funnel separates for the second time; Under 5000r/min, 0 ℃ of condition centrifugal 5 minutes, remove moisture through rotary evaporation;
(4) molecular distillation method preliminary purification mixed fatty acid: the mixing-in fat acid-utilising molecular distillation method separation that the upper step obtains is concentrated, and discard light phase component: distillation condition is scraper plate rotating speed 20r/min, 112 ℃ of temperature of heating plate, pressure 8mtorr;
(5) the urea clathrate method is further extracted purifying alpha-linolenic acid: the envelope solvent is methyl alcohol; Envelope requirement is as follows, and the envelope ratio is lipid acid (g): methyl alcohol (mL): urea (g) is 1:6:2,1:8:1,1:8:2,1:8:3 or 1:10:2, and the envelope temperature is-10 ° of C ~ 30 ° C, and the envelope time is 2 ~ 12h.
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| CN111848341A (en) * | 2020-07-20 | 2020-10-30 | 齐鲁工业大学 | Method for separating and purifying nervonic acid in acer truncatum buge oil by combining molecular distillation with urea inclusion method |
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| 魏决等.酶法从紫苏子油中制取α- 亚麻酸工艺研究(II)尿素包络纯化工艺的探讨.《食品科学》.2005,第26卷(第2期),摘要，第1.3.2节. |
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