CN102746945A - Method for extracting chrysalis oil - Google Patents
Method for extracting chrysalis oil Download PDFInfo
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- CN102746945A CN102746945A CN2011100982317A CN201110098231A CN102746945A CN 102746945 A CN102746945 A CN 102746945A CN 2011100982317 A CN2011100982317 A CN 2011100982317A CN 201110098231 A CN201110098231 A CN 201110098231A CN 102746945 A CN102746945 A CN 102746945A
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Abstract
The invention relates to the technical field of oil production and provides a method for extracting chrysalis oil from silkworm chrysalis by a supercritical fluid extraction technology. The method comprises the following steps of carrying out an extraction process on silkworm chrysalis by a supercritical CO2 fluid at an extraction temperature of 55 DEG C under extraction pressure of 25Mpa, carrying out separation of the extract obtained by the previous step at a separation temperature of 50 to 65 DEG C under separation pressure of 8 to 10Mpa, and collecting a separated liquid which is the chrysalis oil. The method improves an extraction rate of chrysalis oil and alpha-linolenic acid content of chrysalis oil. Azelaic semialdehyde is detected in the chrysalis oil obtained by the method for the first time. The method has a chrysalis oil extraction rate of 33.95% and the chrysalis oil extracted by the method has alpha-linolenic acid content of 67.911%. The chrysalis oil obtained by the method can be used for preparation of drugs and/or health products for diminishing inflammation, resisting allergy, reducing blood fat, reducing blood pressure, reducing blood sugar, resisting aging, preventing myocardial infarction and preventing cerebral infarction.
Description
Technical field
The present invention relates to the grease production technical field, particularly a kind of method that extracts silkworm chrysalis oil.
Background technology
Alpha-linolenic acid is the lipid acid of needed by human; Can be converted into metabolism necessary vital activity factor docosahexenoic acid (DHA) and timnodonic acid (EPA); It is the basic substance that constitutes cytolemma and enzyme; HUMAN HEALTH is played a decisive role, can improve and prevent diseases such as hyperlipidemia, hyperglycemia, hypertension.Alpha-linolenic acid can not synthesize in human body, can only from food, absorb.The product that contains alpha-linolenic acid in the market is many to extract refining forming from perilla oil, Seabuckthorm Seed Oil, butch flax wet goods, but extraction process is complicated, and the content of alpha-linolenic acid is not high.In recent years, often from silkworm chrysalis, extract silkworm chrysalis oil in the industrial production, and then preparation contains the related prods of alpha-linolenic acid.Silkworm chrysalis oil is the mixture that contains multiple higher fatty acid glyceride that from silkworm chrysalis, extract; Outward appearance is the transparent oily liquids of yellow to red; Contain the unsaturated fatty acids that reaches more than 80%, wherein staple is alpha-linolenic acid, oleic acid, linolic acid etc.
At present, the process for extracting of silkworm chrysalis oil mainly contains milling process and solvent extraction method, and milling process divides the press for extracting juice method of making a living, hot moulding method again and boils milling process).The hot moulding method is with to boil the milling process oil yield high, but machine press operation temperature is high, and oxidative rancidity takes place the pufas in the silkworm chrysalis oil easily, influences the quality of oil product; Give birth to good, the lighter color of oil quality that the press for extracting juice method makes, but oil yield is low, Residual oil is high in the dregs of rice.Solvent extraction method extracts grease, the high advantage of the big oil yield of output is arranged, but the solvent usage quantity is big, the difficult control of the dissolvent residual in the product, and also it is not high to extract grease obtained purity.
Supercritical liquid extraction technique (SupereritiealFluidExtraetion; SFE) be a kind of new separation technology; Supercutical fluid is meant that this gas can not liquefy when this state gas pressurization when object was in the above state of its critical temperature (Tc) and emergent pressure (Pc), and just density increases; Character with similar liquids also keeps the performance of gas simultaneously.Supercutical fluid has the advantage of gas and liquid concurrently, and its density approaches liquid, and dissolving power is stronger, and viscosity and gas are close, and spread coefficient helps mass transfer much larger than general liquid.In addition, supercutical fluid has zero surface tension, is easy to permeate in the micropore that is diffused into extract.Therefore, supercutical fluid has good dissolving and mass transfer characteristic, can reach the mass transfer balance soon with extract, realizes effective separation of material.Supercritical liquid extraction technique has the incomparable advantages of traditional technology such as technology is simple, easy to operate; It has not only overcome solvent-extraction process in sepn process; Need the distillation heating; Grease is prone to oxidation, becomes sour, and the defective of dissolvent residual has overcome also that the milling process percentage extraction is low, process for refining is loaded down with trivial details, the unfavorable shortcoming of east of oil.But the supercritical liquid extraction technique that adopts at present extracts silkworm chrysalis oil from silkworm chrysalis, and the extraction temperature and the separation temperature temperature difference are bigger, cause CO
2Exist with the dry ice form, the silkworm chrysalis oil of extraction is because of containing CO
2Dry ice is solid-like, and the percentage extraction of silkworm chrysalis oil is lower, and the yield of alpha-linolenic acid in the silkworm chrysalis oil that finally obtains is reduced.
Summary of the invention
In view of this, the present invention is directed to the defective of existing silkworm chrysalis oil extracting process, propose the supercritical CO of the high silkworm chrysalis oil of a kind of percentage extraction
2Extracting process.This method has reduced the temperature difference of extraction temperature and separation temperature, avoids CO
2Supercutical fluid is solidified into dry ice, has improved the content of alpha-linolenic acid in percentage extraction and the silkworm chrysalis oil of silkworm chrysalis oil.
In order to realize the foregoing invention purpose, the present invention provides following technical scheme:
The invention provides a kind of supercritical CO
2The method of extraction silkworm chrysalis oil is that 55 ℃, extracting pressure are to use supercritical CO under the condition of 25Mpa with silkworm chrysalis in extraction temperature
2Fluid extraction is that 50～65 ℃, separating pressure are to separate under the condition of 8～10Mpa in separation temperature then, collects liquid, obtains silkworm chrysalis oil.
The supercritical fluid extraction sepn process is a relation of utilizing its dissolving power and density, promptly utilizes pressure and temperature that the influence of supercutical fluid dissolving power is carried out.Under supercritical state, fluid contacts with treating isolating material, and it is extracted the heterogeneity of polarity size, boiling point height and molecular mass size selectively successively.Then by decompression or/and the method for cooling makes supercutical fluid become common gases, be extracted material and then separate out fully or basically automatically, thereby reach the purpose of separate purifying.
Extraction temperature influences more complicated to the supercutical fluid dissolving power, and on the one hand, under certain pressure, elevated temperature is because elevated temperature is as extraction agent CO
2Intermolecular distance increase, Intermolecular Forces reduces, density reduces, the corresponding decline of dissolving power; On the other hand, under certain pressure, elevated temperature, the volatility of extract strengthens, the thermal motion of molecule is accelerated, intermolecular form and chance increase, thereby dissolving power is increased.Therefore, temperature to the influence of supercritical extraction rate comprehensively these two factors consider that the present invention selects 55 ℃ of extraction temperature as silkworm chrysalis oil.
Extracting pressure is one of important parameter of supercritical fluid extraction, extraction temperature one timing, and pressure increases, and fluid density increases, and solvent strength strengthens, and the solubleness of solvent increases.After pressure is increased to a certain degree; Then solubleness increases slowly; This be since under the high pressure supercritical phase density with pressure change slowly due to, increase extracting pressure again, the solubleness of solvent raises slowly simultaneously that energy consumption increases; Therefore, select suitable extracting pressure also to have influence for supercritical liquid extraction technique.In the method provided by the invention, select the extracting pressure of 25Mpa as silkworm chrysalis oil.
Supercritical CO when the dissolving silkworm chrysalis oil
2When fluid gets into separator, because the decline of pressure, makes CO or/and variation of temperature
2Thereby become two rapidly with silkworm chrysalis oil and reach isolating purpose mutually.When separation temperature and extraction temperature excessive temperature differentials, CO
2Be prone to be solidified into dry ice, silkworm chrysalis oil thereby one-tenth solid state are stranded in the separator inwall, have reduced the percentage extraction of silkworm chrysalis oil, and then have had influence on the content of alpha-linolenic acid in the silkworm chrysalis oil.In order to prevent extraction temperature and separation temperature excessive temperature differentials, CO
2Dry ice mixes with the silkworm chrysalis oil of extraction, influences the percentage extraction and the quality of silkworm chrysalis oil, and it is that 50～65 ℃, separating pressure are to separate supercritical CO under the condition of 8～10Mpa that method provided by the invention is employed in separation temperature
2Fluid and the grease that from silkworm chrysalis, extracts are collected liquid, obtain silkworm chrysalis oil.
As preferably, in the method provided by the invention, be separated under 50 ℃ and carry out.
Preferably, in the method provided by the invention, be separated under the 8Mpa and carry out.
In order fully to extract the silkworm chrysalis oil in the silkworm chrysalis, method provided by the invention also is included in carries out secondary separation under 35～55 ℃.
Preferably, in the method provided by the invention, secondary separation is carried out under 35 ℃.
As preferably, in the method provided by the invention, secondary separation is carried out under the pressure of 4～6Mpa.
Preferably, in the method provided by the invention, secondary separation is carried out under 4Mpa.
Supercritical CO
2The influence of flow rate of fluid and extraction time: in the supercritical fluid extraction process, the flow of extraction agent mainly influences the extraction time.In general, yield one timing, flow is big more, and the heat transmission resistance between solvent, solute is more little, and then the speed of extraction is fast more, and the needed extraction time is short more, but extraction is reclaimed load greatly.One timing of extraction agent flow, the extraction time is long more, and yield is high more.During the extraction beginning, because solvent does not reach good with solute and contacts, yield is lower.Along with the lengthening of extraction time, extraction rate increases, and after reaching maximum, owing to treat the minimizing of separated portion, mass transfer power reduces and extraction rate is reduced.Along with the increase of extraction time, yield increases gradually, and as time passes, yield increases significantly, and reaching certain hour increases slowly afterwards.For raising the efficiency, save energy should be taken all factors into consideration and select suitable extraction time and flow.The present invention selects to feed the CO that flow is 25kg/h
2, the extraction time is 3～5h.
As preferably, in the method provided by the invention, the extraction time of silkworm chrysalis oil is 4h.
The big I of extraction particulate influences percentage extraction, and generally speaking, granularity is more little; Diffusion time is short more, helps supercutical fluid to the material internal migration, has increased mass transfer effect; Not only can seriously stop up sieve aperture but the material pulverizing is meticulous; Cause the obstruction of extractor egress filtering net, and can increase the surface flow resistance, be unfavorable for extraction on the contrary.Moisture also is the important factor that influences extraction efficiency; When water cut is higher in the material; Its moisture mainly forms continuous system with unit molecule moisture film form at wetting ability macromole interface, thereby has increased supercritical phase mobile resistance, when continuing to moisturize; Redundant moisture mainly exists with free state, and extraction is not produced tangible influence.And when water cut was low, water molecules mainly existed with discrete unimolecular layer form.It is thus clear that, destroy the continuous moisture film at mass transfer interface, make between solute and the solvent effectively to contact, form the influence that successive main body mass transfer system just can reduce moisture.In order to guarantee silkworm chrysalis and supercritical CO
2Fluid fully contacts, and improves the extraction yield of silkworm chrysalis oil, and method provided by the invention also comprises carries out drying and crushing to silkworm chrysalis, crosses the pre-treatment of 40 mesh sieves, to improve percentage extraction.
Particularly, the present invention adopts supercritical CO
2The extraction silkworm chrysalis oil with the silkworm chrysalis drying and crushing, is crossed 40 mesh sieves, evenly is placed in the extraction kettle effusive CO from steel cylinder
2Through after purifying, get into condenser condenses and become liquid, be forced into extracting pressure 25Mpa through HPP, again after heating unit is heated to 55 ℃ of extraction temperature, CO
2Become supercutical fluid, get into the silkworm chrysalis bed of flowing through from extraction kettle bottom, contact with the silkworm chrysalis raw material, dissolving grease wherein gets into separation reactor I, separation reactor I I and reduces pressure step by step after the cooling when being dissolved with greasy fluid, because of CO
2Dissolving power descends, the same CO of grease
2Separate, emit CO from the separating still bottom
2Get into condensing surface liquefaction through cleaner, recycle.Separation reactor I is a flash trapping stage, and separation condition is 50～65 ℃, 8～10Mpa; Separation reactor I I is that secondary separates, and separation condition is 35～55 ℃, 4～6Mpa.
Preferably, the present invention adopts supercritical CO
2The extraction silkworm chrysalis oil with the silkworm chrysalis drying and crushing, is crossed 40 mesh sieves, evenly is placed in the extraction kettle effusive CO from steel cylinder
2Through after purifying, get into condenser condenses and become liquid, be forced into extracting pressure 25Mpa through HPP, again after heating unit is heated to 55 ℃ of extraction temperature, CO
2Become supercutical fluid, get into the silkworm chrysalis bed of flowing through from extraction kettle bottom, contact with the silkworm chrysalis raw material, dissolving grease wherein gets into separation reactor I, separation reactor I I and reduces pressure step by step after the cooling when being dissolved with greasy fluid, because of CO
2Dissolving power descends, the same CO of grease
2Separate, emit CO from the separating still bottom
2Get into condensing surface liquefaction through cleaner, recycle.Separation reactor I is a flash trapping stage, and separation condition is 50 ℃, 8Mpa; Separation reactor I I is that secondary separates, and separation condition is 35 ℃, 4Mpa.
The present invention also provides above-mentioned supercritical CO
2The silkworm chrysalis oil that extraction process obtains.
The present invention also provides above-mentioned supercritical CO
2The application of the silkworm chrysalis oil that extraction process obtains in preparation anti-inflammatory, reducing blood-fat, hypotensive, hypoglycemic drug and/or healthcare products.
Supercritical CO provided by the invention
2Extraction process extracts silkworm chrysalis oil from silkworm chrysalis, use supercritical fluid extraction, because whole process is without organic solvent, so extract do not have residual vehicle substance, has avoided the existence of harmful thing in the leaching process and to the pollution of environment; Extraction and sepn process combine, as the CO of saturated solute
2When fluid gets into separator, because the decline or the variation of temperature of pressure, make CO
2With extract become rapidly two mutually (gas-liquid separation) separate, extraction efficiency height and energy consumption are less, have improved production efficiency and have also reduced production cost.The percentage extraction of silkworm chrysalis oil is 33.95%.Utilize supercritical CO provided by the invention
2Extraction process extracts silkworm chrysalis oil from silkworm chrysalis, carry out at normal temperatures, and is easy and simple to handle, and the grease that extracts has kept natural nutrition and biological activity, and do not have aldehyde, ketone peculiar smell, and organic solvent-free is residual, and human body safety is not had harm.After silkworm chrysalis oil is prepared into mixed fatty acid, through the Pottasium Hydroxide saponification, esterification in the presence of boron trifluoride-methanol; (GC-MS) analyzes the composition in the silkworm chrysalis oil with gas chromatography-mass spectrography; Test-results shows that alpha-linolenic acid content is 67.911% in the silkworm chrysalis oil that makes, so the silkworm chrysalis oil that the present invention extracts from silkworm chrysalis can improve immune function of human body; The delaying human body function is old and feeble, reducing blood-fat, decreasing cholesterol, to the treatment hypercholesterolemia with improve liver function remarkable effect is arranged.Test-results shows that silkworm chrysalis oil provided by the invention has remarkable prevention and therapeutic action to fat hepatitis.Therefore, supercritical CO provided by the invention
2The silkworm chrysalis oil that extraction process makes can be used in preparation anti-inflammatory, antianaphylaxis, reducing blood-fat, hypotensive, hypoglycemic, anti-ageing, prevention myocardial infarction, prevention of brain infarct medicine and/or healthcare products.
Description of drawings
Fig. 1 shows the technical process of supercritical fluid extraction extraction silkworm chrysalis oil.
Fig. 2 show silkworm chrysalis oil that the present invention makes change into lipid acid after gas chromatography mass spectrometry detect collection of illustrative plates.
Fig. 3 shows the form of liver tissues of rats in the animal experiment normal control group.Rats in normal control group normal diet drinking-water.
Fig. 4 shows the form of liver tissues of rats in the animal test model group.The model group rat is except that normal diet drinking-water, and every morning gives the 1mL lipomul according to the 100g body weight and irritates 6 weeks of stomach.
Fig. 5 shows the form of liver tissues of rats in the low dose of test group of animal experiment (2mg/kg).Low dose of rats in test groups is except that normal diet drinking-water, and every morning gives 1mL lipomul according to the 100g body weight, irritates stomach after 6 weeks, and give silkworm chrysalis oil that 2mg the present invention make according to the 1kg body weight every afternoon, 4 weeks of administration.The experiment end stopped to give lipomul in preceding 3 days, continued administration.After the off-test, water is can't help in rat fasting overnight, and anesthesia is got right lobe of liver and is organized in 4% the Superlysoform fixing.
Fig. 6 shows the form of liver tissues of rats in the heavy dose of test group of animal experiment (4mg/kg).Heavy dose of rats in test groups is except that normal diet drinking-water, and every morning gives 1mL lipomul according to the 100g body weight, irritates stomach after 6 weeks, and give silkworm chrysalis oil that 4mg the present invention make according to the 1kg body weight every afternoon, 4 weeks of administration.The experiment end stopped to give lipomul in preceding 3 days, continued administration.After the off-test, water is can't help in rat fasting overnight, and anesthesia is got right lobe of liver and is organized in 4% the Superlysoform fixing.
Fig. 7 shows the form of liver tissues of rats in the positive drug control group (rosiglitazone 4mg/kg).The positive drug control rats is except that normal diet drinking-water, and every morning gives 1mL lipomul according to the 100g body weight, irritates stomach after 6 weeks, and give 4mg rosiglitazone according to the 1kg body weight every afternoon, 4 weeks of administration.The experiment end stopped to give lipomul in preceding 3 days, continued administration.After the off-test, water is can't help in rat fasting overnight, and anesthesia is got right lobe of liver and is organized in 4% the Superlysoform fixing.
Embodiment
The invention discloses a kind of supercritical extraction method of silkworm chrysalis oil, those skilled in the art can use for reference this paper content, suitably improve processing parameter and realize.Special needs to be pointed out is that all similarly replace and change apparent to those skilled in the art, they all are regarded as and are included in the present invention.Method of the present invention and application are described through preferred embodiment; The related personnel obviously can change or suitably change and combination methods and applications as herein described in not breaking away from content of the present invention, spirit and scope, realizes and use technology of the present invention.
The invention provides a kind of supercritical CO
2The method of extraction silkworm chrysalis oil is that 55 ℃, extracting pressure are to use supercritical CO under the condition of 25Mpa with silkworm chrysalis in extraction temperature
2Fluid extraction is in order to prevent extraction temperature and separation temperature excessive temperature differentials, CO
2Dry ice mixes with the silkworm chrysalis oil of extraction, influences the percentage extraction and the quality of silkworm chrysalis oil, and it is that 50～65 ℃, separating pressure are to separate supercritical CO under the condition of 8～10Mpa that method provided by the invention is employed in separation temperature
2Fluid and the grease that from silkworm chrysalis, extracts are collected liquid, obtain silkworm chrysalis oil.
Preferably, be separated in 50 ℃, carry out under the 8Mpa.
As preferably, also be included in and carry out secondary separation under 35～55 ℃.
As preferably, secondary separation is carried out under the pressure of 4～6Mpa.
Preferably, secondary separation is carried out under the 4Mpa at 35 ℃.
As preferably, supercritical CO
2The fluidic flow is 25kg/h.
As preferably, the time of extraction is 3～5h.
As preferably, also comprise the step of drying and crushing silkworm chrysalis.
The silkworm chrysalis main body of oil is alpha-linolenic acid, oleic acid, linolic acid etc.Wherein, the alpha-linolenic acid chemical name: all-cis formula-9,12,15-punicic acid (Allcis-9,12,15-Octadecatrienoic acid), the expression symbol is 18:3 Δ 9,12,15 or 18:3n-3, ω-3.Its chemical structure is following:
Alpha-linolenic acid is colourless extremely light yellow tasteless oily liquids, is dissolved in ethanol and ether, and is water insoluble.Fusing point is 10～11.3 ℃, and boiling point is 224.5 ℃/1.3kPa, and specific density is 0.9157g/cm
3, specific refractory power is 1.4800.Alpha-linolenic acid is the pufas that contains 3 ethylene linkages, and is very easily oxidized in the repeated heating of general milling process and solvent method and sepn process, degrade.
Alpha-linolenic acid mainly directly absorbs through enteron aisle, stores at liver, is transported to each position of health through blood, directly becomes the structural material of cytolemma; Secondly; Alpha-linolenic acid is the parent of pufas as ω-3; Prolong in carbochain under the effect of enzyme and desaturase; Prolong with desaturation and can metabolism produce multiple high reactivity material through carbochain, regulation and control body biochemical reaction increases intelligence, vision protection, inhibition are old and feeble, inhibition anaphylaxis and thrombotic diseases, reduce fat, lowering blood glucose, the generation that brings high blood pressure down, suppresses cancer and transfer, prevention myocardial infarction and cerebral infarction, anti-inflammatory action etc.
Alpha-linolenic acid is to the effect of cardiovascular disorder: discover, take the 3g alpha-linolenic acid every day, can improve the level of timnodonic acid in the blood plasma (EPA) and docosahexenoic acid (DHA), thereby reach the purpose of prevention and treatment cardiovascular and cerebrovascular diseases; Alpha-linolenic acid can also change into thromboxane A through antithrombotic, inhibition arachidonic acid
2, avoid the generation of myocardial infarction.
Antitumous effect: discover that alpha-linolenic acid can reduce the incidence of mammary cancer, carcinoma of the pancreas, colorectal carcinoma and tumor of kidney, suppress growth of tumor, its mechanism of action is the expression that has reduced insulin-like growth factor I and Urogastron.
Anti-inflammatory, anti-allergic effects: the research proof, alpha-linolenic acid can reduce the content of arachidonic acid (AA) in multinuclear leucocyte (RMNS) and the mastocyte membrane phospholipid, and the arachidonic acid burst size reduced when anaphylaxis was taken place, and generated thereby reduce LT4 (leukotriene); The meta-bolites timnodonic acid of alpha-linolenic acid also has the effect with arachidonic acid competition desaturase, reduces the generation of inflammatory reaction; Alpha-linolenic acid has restraining effect to anaphylaxis midbody platelet aggregation activation factor (RAF), and therefore, alpha-linolenic acid has the inhibition effect to anaphylaxis and inflammation.
Discovering that the reducing blood lipid of alpha-linolenic acid is realized through the adjusting to metabolic rate on the one hand, then is to realize through suppressing relevant fat and glycerine synthetase series and cholesterol synthase on the other hand.Alpha-linolenic acid can make the activity of the rate-limiting enzyme 3-Hydroxy-3-methylglutaryl CoA A (HMG-CoA) of cholesterol synthase reduce and the generation of minimizing SUV; Alpha-linolenic acid increases the synthetic minimizing of triglyceride level, consumption to the inhibition of lipese system (comprising fatty acid synthetase, coenzyme A-carboxylase, diacylglycerol Transacetylase etc.) and the β-Yang Hua in the line feeder plastochondria.Alpha-linolenic acid suppresses the metabolism that ω-6 is pufas (PUFA) through competitive inhibitory effect; Reduce the synthetic of Prostaglandin PGE2, prostacyclin PGI2, thromboxane TXA2, leukotriene LT4; Increasing corresponding ω-3 is the meta-bolites of pufas (PUFA); Thereby produce numerous biological regulating and controlling effects, like anti-inflammatory, antithrombotic, antianaphylaxis etc.
Suppress old and feeble: modern medicine thinks that radical is to cause one of old and feeble important factor.Active oxygen and other radicals pair cell as a rule have the overt toxicity effect, as cause nucleic acid, protein, fat, carbohydrate and microbial film sex change, and disorganization is with aging.One of Radical Metabolism product is mda (MDA), and its content can reflect the oxidized degree of cell, and superoxide-dismutase (SOD) passes through O
2 -Play the synthetic H of disproportionation
2O
2, become water by the continuous metabolism of other antioxidases again, remove radical.Research shows that alpha-linolenic acid can obviously reduce mda content in brain and the liver, obviously improves the vigor of superoxide-dismutase simultaneously, and alpha-linolenic acid has good anti-aging effects.
To visual acuity affected: discover,, can improve the level of the omega-3 polyunsaturated fatty acids DNA on the visual cell adventitia, the electrical potential activity in the electroretinogram is strengthened through increasing the alpha-linolenic acid in the meals.
Antiobesity action: alpha-linolenic acid can increase metabolic rate or suppress the synthetic of triglyceride, increases the drainage of various lipids in the body.
Simultaneously, alpha-linolenic acid has very high security to human body, discovers, in the acute and chronic toxicological experiment of mouse, irritates stomach 90 days with 1.5g/dkg, and not seeing has any toxic reaction.Supercritical CO provided by the invention
2The silkworm chrysalis oil that extraction process obtains is because be rich in alpha-linolenic acid, can be used to prepare anti-inflammatory, reducing blood-fat, hypotensive, hypoglycemic drug and/or healthcare products.
As preferably, the present invention also provides above-mentioned supercritical CO
2The application of the silkworm chrysalis oil that extraction process obtains in preparation anti-inflammatory drug and/or healthcare products.
Fat hepatitis specifically refers to be secondary to the hepatitis that bulla property liver cell fat becomes, and can fat hepatitis be divided into alcoholic hepatitis and nonalcoholic fatty liver disease two big classes according to the cause of disease.Both liver histologicals change similar basically, all show as on adipohepatic basis, ballooning degeneration of liver cells occurs, and neutrophil leucocyte is main Combination inflammatory cell infiltration in the leaflet.The part fat hepatitis is still with fibrosis around horse Lip river mile (Mallory) corpusculum and cell peripheral fibrosis and the central vein.
Preferably, the present invention also provides above-mentioned supercritical CO
2The application of the silkworm chrysalis oil that extraction process obtains in preparation treatment fat hepatitis medicine and/or healthcare products.
Supercritical CO provided by the invention
2Extraction process extracts silkworm chrysalis oil from silkworm chrysalis, the percentage extraction of silkworm chrysalis oil is 33.95%.Utilize supercritical CO provided by the invention
2Extraction process extracts silkworm chrysalis oil from silkworm chrysalis, carry out at normal temperatures, and is easy and simple to handle, and the grease that extracts has kept natural nutrition and biological activity, and do not have aldehyde, ketone peculiar smell, and organic solvent-free is residual, and human body safety is not had harm.
Analyzing Ester method commonly used is it to be derived be carboxylates such as volatile methyl esters, uses gas chromatography-mass spectrography (GC-MS) to measure then.After the present invention was prepared into mixed fatty acid with silkworm chrysalis oil, through the Pottasium Hydroxide saponification, esterification in the presence of boron trifluoride-methanol detected with the gas chromatography mass spectrometry system then.Therefore, the present invention adopts gas chromatography-mass spectrography (GC-MS) that the composition in the silkworm chrysalis oil is analyzed.After silkworm chrysalis oil is prepared into mixed fatty acid; Through the Pottasium Hydroxide saponification, esterification in the presence of boron trifluoride-methanol, (GC-MS) analyzes the composition in the silkworm chrysalis oil with gas chromatography-mass spectrography; Test-results shows that alpha-linolenic acid content is 67.911% in the silkworm chrysalis oil that makes.
Among the present invention, silkworm chrysalis is focused the consruction on subject by University Of Suzhou's medical board preclinical medicine and bio-science institute the 211 Project---and silkworm heredity research department in the rain provides.
Below in conjunction with embodiment, further set forth the present invention:
Accurately take by weighing the wet silkworm chrysalis of 1051.2g, put into the dry 48h of 70 ℃ of gas blowers, the sterilization postposition tells kibbler to pulverize, and crosses 40 mesh sieves, and is subsequent use.
Open the supercritical fluid extraction equipment power supply, open refrigeration, cold circulation, the temperature of extraction kettle temperature regulating device is adjusted to 55 ℃, the temperature of separation reactor I temperature regulating device is adjusted to 50 ℃, and separation reactor I I temperature regulating device is adjusted to 35 ℃.The silkworm chrysalis of crushing screening is packed into behind the barrel, put into extraction kettle, install sealing-ring, the plug of screwing.After the temperature of treating extraction kettle, separation reactor I, separation reactor I I reaches design temperature, open CO
2Steel cylinder is opened HPP, pressurizes; After extraction kettle pressure is near 25Mpa, open the valve between extraction kettle, separation reactor I, the separation reactor I I, pressurize step by step; Pressure remains on 25Mpa in the extraction kettle to making to treat pressure equilibrium, and separation reactor I pressure is 8Mpa, when separation reactor I I pressure is 4Mpa; Open the loop valve, system is formed reflux.Behind the extraction 3.5h, collect silkworm chrysalis oil from separation reactor I, separation reactor I I discharge port respectively.
Embodiment 2 supercritical fluid extraction extraction silkworm chrysalis oils according to the invention
Accurately take by weighing the wet silkworm chrysalis of 1060.0g, put into the dry 48h of 70 ℃ of gas blowers, the sterilization postposition tells kibbler to pulverize, and crosses 40 mesh sieves, and is subsequent use.
Open the supercritical fluid extraction equipment power supply, open refrigeration, cold circulation, the temperature of extraction kettle temperature regulating device is adjusted to 55 ℃, the temperature of separation reactor I temperature regulating device is adjusted to 46 ℃, and separation reactor I I temperature regulating device is adjusted to 41 ℃.The silkworm chrysalis of crushing screening is packed into behind the barrel, put into extraction kettle, install sealing-ring, the plug of screwing.After the temperature of treating extraction kettle, separation reactor I, separation reactor I I reaches design temperature, open CO
2Steel cylinder is opened HPP, pressurizes; After extraction kettle pressure is near 25Mpa, open the valve between extraction kettle, separation reactor I, the separation reactor I I, pressurize step by step; Pressure remains on 25Mpa in the extraction kettle to making to treat pressure equilibrium, and separation reactor I pressure is 10Mpa, when separation reactor I I pressure is 6Mpa; Open the loop valve, system is formed reflux.Behind the extraction 3h, collect silkworm chrysalis oil from separation reactor I, separation reactor I I discharge port respectively.
Accurately take by weighing the wet silkworm chrysalis of 1050.0g, put into the dry 48h of 70 ℃ of gas blowers, the sterilization postposition tells kibbler to pulverize, and crosses 40 mesh sieves, and is subsequent use.
Open the supercritical fluid extraction equipment power supply, open refrigeration, cold circulation, the temperature of extraction kettle temperature regulating device is adjusted to 55 ℃, the temperature of separation reactor I temperature regulating device is adjusted to 65 ℃, and separation reactor I I temperature regulating device is adjusted to 55 ℃.The silkworm chrysalis of crushing screening is packed into behind the barrel, put into extraction kettle, install sealing-ring, the plug of screwing.After the temperature of treating extraction kettle, separation reactor I, separation reactor I I reaches design temperature, open CO
2Steel cylinder is opened HPP, pressurizes; After extraction kettle pressure is near 25Mpa, open the valve between extraction kettle, separation reactor I, the separation reactor I I, pressurize step by step; Pressure remains on 25Mpa in the extraction kettle to making to treat pressure equilibrium, and separation reactor I pressure is 9Mpa, when separation reactor I I pressure is 5Mpa; Open the loop valve, system is formed reflux.Behind the extraction 5h, collect silkworm chrysalis oil from separation reactor I, separation reactor I I discharge port respectively.
Accurately take by weighing the wet silkworm chrysalis of 1058.0g, put into the dry 48h of 70 ℃ of gas blowers, the sterilization postposition tells kibbler to pulverize, and crosses 40 mesh sieves, and is subsequent use.
Open the supercritical fluid extraction equipment power supply, open refrigeration, cold circulation, the temperature of extraction kettle temperature regulating device is adjusted to 55 ℃, the temperature of separation reactor I temperature regulating device is adjusted to 52 ℃, and separation reactor I I temperature regulating device is adjusted to 43 ℃.The silkworm chrysalis of crushing screening is packed into behind the barrel, put into extraction kettle, install sealing-ring, the plug of screwing.After the temperature of treating extraction kettle, separation reactor I, separation reactor I I reaches design temperature, open CO
2Steel cylinder is opened HPP, pressurizes; After extraction kettle pressure is near 25Mpa, open the valve between extraction kettle, separation reactor I, the separation reactor I I, pressurize step by step; Pressure remains on 25Mpa in the extraction kettle to making to treat pressure equilibrium, and separation reactor I pressure is 8Mpa, when separation reactor I I pressure is 4Mpa; Open the loop valve, system is formed reflux.Behind the extraction 4h, collect silkworm chrysalis oil from separation reactor I, separation reactor I I discharge port respectively.
The calculating and the attributional analysis of embodiment 5 silkworm chrysalis oil percentage extractions according to the invention
Calculate grease extraction yield (%)=extraction oil weight/example weight * 100.
Table 1 silkworm chrysalis oil percentage extraction
Silkworm chrysalis oil to making among the embodiment 1 to 4 carries out mass analysis, and the result is as shown in table 2.
The quality index of table 2 silkworm chrysalis oil
| Index name | Index |
| Outward appearance | Faint yellow oily liquids to yellow transparent |
| Smell | The distinctive fragrance of tool silkworm chrysalis, positive constant error free from extraneous odour |
| Color and luster (Pt-Co colorimetric number) | ≤300 |
| Acid number (mg KOH/g) | ≤0.2 |
| Iodine number (gI 2/100g) | 130～138 |
| Saponification value (mg KOH/g) | 191～195 |
| Proportion (20/4 ℃) | 0.914～0.918 |
| Moisture and volatile matter content | ≤0.1 |
| Impurity | ≤0.1 |
The silkworm chrysalis oil that embodiment 1 to 4 extract is the mixture that contains multiple lipid acid, and it is light to the transparent oily liquids of xanchromatic, water insoluble that outward appearance is, but dissolve in organic solvents such as gasoline, acetone, benzene and sherwood oil.The distinctive fragrance of tool silkworm chrysalis, free from extraneous odour, quality is better.
The preparation of silkworm chrysalis oil mixed fatty acid: take by weighing silkworm chrysalis oil 15g that embodiment 1 to 4 makes respectively in round-bottomed flask; Add 4%NaOH ethanolic soln 60mL, 1h is stirred in 65 ℃ of waters bath with thermostatic control, is cooled to room temperature; It is saponified to add water to the clarification dissolving, adds a small amount of petroleum ether extraction unsaponifiables again.Water intaking layer adds 1 times of water yield dilution, and adding 10% HCl again, to regulate pH value be 3～4, use petroleum ether extraction, merges extremely neutrality of organic phase and washing, with reclaim under reduced pressure sherwood oil behind the anhydrous sodium sulfate drying, promptly gets mixed fatty acid.The average of the extraction yield of mixed fatty acid is 91.0%.
Esterification: accurately take by weighing the silkworm chrysalis oil mixed fatty acid 0.4g that makes respectively; Add 0.5mol/L Pottasium Hydroxide-methyl alcohol 3mL, put 60 ℃ of water-bath 15min～30min (to the oil droplet completely dissolve), add 14% boron trifluoride-methanol 2mL after the cooling; Put 60 ℃ of water-bath 5min; Add normal hexane 2mL after the cooling, saturated nacl aqueous solution 2mL, centrifugal layering.Get supernatant, it is subsequent use to add anhydrous sodium sulfate drying.
Chromatographic condition is set: the Hp-5 capillary column; Carrier gas N
2Press 49kPa before the post; 270 ℃ of injector temperatures; 250 ℃ of transmission line temperature; 200 ℃ of ion source temperatures; Temperature programming: ℃ (5min) → 20,130 ℃ → 10 ℃/min → 185 ℃/℃ (2min) → 50, min → 220 ℃/min → 285 ℃ (10min); Sweep velocity: 500u/s, ionization mode: 70eV, mass scanning scope: 20AMU～380AMU.
GC-MS analyzes: with the normal hexane is solvent, and esterification silkworm chrysalis lipid acid (200mg/mL) is made into the solution that concentration is 10 μ g/ μ L, and sample introduction 1 μ L is provided with parallel test.Mass-spectrometric data according to document and NIST/EPA/NIH spectrum storehouse is retrieved, and identifies the lipid acid in the silkworm chrysalis oil, and according to DPS the peak area of chromatographic peak is carried out normalization method and handle, and the result sees table 3.
Table 3GC-MS analyzes the silkworm chrysalis oil fatty acid component
The result shows, the silkworm chrysalis oil stable components, and main active substances alpha-linolenic acid average content is 67.911%.Wherein aldehydo caprylic acid is a detected composition from silkworm chrysalis oil first.
Male cleaning level SD rat, body weight 230～250g, totally 50 are adopted in test.Rat is divided into groups; Being divided into is 5 groups, is respectively normal control group, model group (lipomul), heavy dose of test group (the silkworm chrysalis oil 4mL/kg that lipomul+embodiment 1 makes), low dose of test group (the silkworm chrysalis oil 2mL/kg that lipomul+embodiment 1 makes) and mixed fatty acid control group (lipomul+lipid acid mixed solution 4mg/kg), 10 every group; Experimental animal ad lib and drinking-water; Except that rats in normal control group, all the other rats equal every mornings presses the 1mL/100g body weight with lipomul and irritates 6 weeks of stomach, wherein; The lipomul composition is seen table 4, and lipid acid mixed solution composition is seen table 5.
After 6 weeks, except that the normal control group, model group, test group and control group continue to give lipomul the morning, and afternoon, each administration group gave the medicine of each respective concentration, 4 weeks of administration.The experiment end stopped to give lipomul in preceding 3 days, but continued administration.Before experiment finished, water was can't help in rat fasting overnight, anesthesia, and abdominal aortic blood, each is organized rat and leaves and takes an amount of tissue preparation 20% liver tissue homogenate's liquid in the left lobe of liver same area; Other gets right lobe of liver same area tissue, and is fixing in 4% Superlysoform.The lipomul prescription is seen table 4.
Lipomul prescription in table 4 animal experiment
| Composition | Unit | Content |
| Semen Maydis oil (Corn oil) | (g) | 400 |
| Sucrose (Saccharose) | (g) | 150 |
| Whole milk powder (Total milk powder) | (g) | 80 |
| SUV (Cholesterol) | (g) | 100 |
| Sodium desoxycholate (Sodium deoxycholate) | (g) | 10 |
| Tween-80 (Tween 80) | (g) | 36.4 |
| Ucar 35 (Propylene glycol) | (g) | 31.1 |
| Compound vitamin b6 usp (Vitamin mixture) | (g) | 2.5 |
| Salt (Cooking salt) | (g) | 10 |
| Mineral substance (Mineral mixture) | (g) | 1.5 |
| Zero(ppm) water (Distilled water) | (mL) | 300 |
| Total energy (Total energy) | (kcal/L) | 4342 |
The silkworm chrysalis oil fatty acid component that the present invention who records according to GC-MS makes, preparation lipid acid mixed solution, moity is seen table 5.
Table 5 mixed fatty acid is formed
| The component numbering | Component | Relative content (%) |
| 1 | Aldehydo caprylic acid (Azelaic semialdehyde) | 0.026 |
| 2 | Lauric acid (Dodecanoic acid) | 0.089 |
| 3 | Tetradecanoic acid (Myristic acid) | 0.176 |
| 4 | 15 carbonic acid (Pentadecyclic acid) | 0.034 |
| 5 | Palm diluted acid (Palmitoleic acid) | 0.960 |
| 6 | Palmiticacid (Palmitic acid) | 26.796 |
| 7 | Oleic acid (Oleic acid) | 0.143 |
| 8 | Alpha-linolenic acid (α-linolenic acid) | 31.725 |
| 9 | Triple Pressed Stearic Acid (Stearic acid) | 3.541 |
| 10 | Zero(ppm) water (Distilled water) | 36.186 |
Testing index: hepatic tissue is weighed and is calculated the heavy coefficient of liver; Separation of serum; Measure serum total cholesterol (TC), triglyceride level (TG), RHDL (HDL-C), free fatty acids (FFA), gpt (ALT) and glutamic-oxal(o)acetic transaminase (AST) according to ordinary method respectively, and by formula calculate low-density lipoprotein (LDL-C) (LDL-C=TC-TG/2.2-HDL-C); 20% liver tissue homogenate's liquid is measured hepatic tissue TC, TG, FFA, superoxide-dismutase (SOD) and reduced glutathion (GSH) according to ordinary method; The hepatic tissue of 4% formalin fixed is done morphologic detection.Detected result is seen table 6.
Table 6 silkworm chrysalis oil and lipid acid mixed solution effect are relatively
Compare with the normal control group,
△Expression P＜0.05,
△ △Expression P＜0.01; Compare with model group,
*Expression P＜0.05.
*Expression P＜0.01.
Male cleaning level SD rat, body weight 230～250g, totally 50 are adopted in test.Rat experiment is divided into groups; Be divided into is 5 groups; Be respectively normal control group, model group (lipomul), heavy dose of test group (the silkworm chrysalis oil 34mL/kg that makes among lipomul+embodiment 3), low dose of test group (the silkworm chrysalis oil 32mL/kg that makes among lipomul+embodiment 3) and positive drug control group (lipomul+rosiglitazone 4mg/kg); Every group 10; Experimental animal ad lib and drinking-water, except that rats in normal control group, all the other rats equal every mornings presses the 1mL/100g body weight with lipomul and irritates 6 weeks of stomach.
After 6 weeks, except that the normal control group, model group, test group and positive drug control group continue to give lipomul the morning, and afternoon, each administration group gave the medicine of each respective concentration, 4 weeks of administration.The experiment end stopped to give lipomul in preceding 3 days, but continued administration.Before experiment finished, water was can't help in rat fasting overnight, anesthesia, and abdominal aortic blood, each is organized rat and leaves and takes an amount of tissue preparation 20% liver tissue homogenate's liquid in the left lobe of liver same area; Other gets right lobe of liver same area tissue, and is fixing in 4% Superlysoform.The lipomul prescription is seen table 4 among the embodiment 8.
Testing index: separation of serum; Measure serum total cholesterol (TC), triglyceride level (TG), RHDL (HDL-C), free fatty acids (FFA), gpt (ALT) and glutamic-oxal(o)acetic transaminase (AST) respectively, and by formula calculate low-density lipoprotein (LDL-C) (LDL-C=TC-TG/2.2-HDL-C); 20% liver tissue homogenate's liquid is measured hepatic tissue superoxide-dismutase (SOD) and reduced glutathion (GSH), and the result sees table 7.
Table 7 silkworm chrysalis oil is to the influence of high fat diet inductive fat hepatitis rat each item index
Compare with the normal control group,
△Expression P＜0.05,
△ △Expression P＜0.01; Compare with model group,
*Expression P＜0.05,
*Expression P＜0.01.
Compare with the normal control group, rat gives lipomul after 10 weeks, and model group Serum TC, TG, HDL-C, LDL-C and FFA content all have significance rising (P＜0.01); And compare with model group; The high fat diet rat gives silkworm chrysalis oil 4mL/kg and 2mL/kg respectively after 4 weeks; Serum TC, TG, HDL-C, LDL-C and FFA all have reduction (P＜0.01 or P＜0.05) in various degree, and positive drug rosiglitazone group rat blood serum These parameters also has improve (P＜0.01 or P＜0.05) in various degree.
With the normal control group relatively, give 10 weeks of high fat diet after, model group rat blood serum ALT and AST, and liver SOD content do not see that all considerable change is arranged, and liver reduced glutathion content has obvious decline (P＜0.05); With model group relatively, each administration group rat blood serum ALT and AST, and liver SOD content also do not see that considerable change is arranged, and the silkworm chrysalis oil heavy dose high fat diet rat liver reduced glutathion content (P＜0.05) that can obviously raise.
Testing index: hepatic tissue is weighed and is calculated the heavy coefficient of liver; 20% liver tissue homogenate's liquid is measured hepatic tissue TC, TG, FFA liver lipid index.
Table 8 silkworm chrysalis oil is to the influence of high fat diet inductive fat hepatitis rat dry weight coefficient and liver tissue homogenate's each item index
Compare with the normal control group,
△Expression P＜0.05,
△ △Expression P＜0.01; Compare with model group,
*Expression P＜0.05,
*Expression P＜0.01.
Compare with the normal control group, the heavy coefficient of the liver of model group rat has significance to increase (P＜0.01), and significance increases liver TC and TG content (P＜0.01), the obvious simultaneously content (P＜0.01) that reduces FFA in the liver; Compare with model group; After the high fat diet rat gives silkworm chrysalis oil; The heavy coefficient of rats'liver, liver TC, TG and FFA content all have some improvement, but do not see that statistical significance is arranged, and positive drug rosiglitazone group rat These parameters all has relatively good effect (P＜0.01 or P＜0.05).
Morphologic detection: the hepatic tissue of 4% formalin fixed is done morphologic detection, and the result sees Fig. 3 to Fig. 7.Silkworm chrysalis oil is seen table 9 to the influence of high fat diet inductive fat hepatitis liver tissues of rats pathological change.
Table 9 silkworm chrysalis oil is to the influence of high fat diet inductive fat hepatitis liver tissues of rats pathological change
Compare P＜0.05, P＜0.01 with model group.
Hepatic tissue morphologic detection result shows: rats in normal control group hepatic tissue structural integrity, and the liver rope is high-visible, and not seeing has lipid cavity, cell infiltration and necrosis region etc.; And the model group liver tissues of rats contains a large amount of lipid cavitys, and with a large amount of cell infiltration, and after giving the various dose silkworm chrysalis oil, liver lipid cavity and inflammatory cell all have certain improvement effect, wherein, the effect of silkworm chrysalis oil 4mL/kg group is better.
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; Can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.
Claims (7)
1. a method that extracts silkworm chrysalis oil is characterized in that, is that 55 ℃, extracting pressure are to use supercritical CO under the condition of 25Mpa with silkworm chrysalis in extraction temperature
2Fluid extraction is that 50～65 ℃, separating pressure are to separate under the condition of 8～10Mpa in separation temperature then, collects liquid, obtains silkworm chrysalis oil.
2. the method for claim 1 is characterized in that, the said separation temperature that is separated in is 50 ℃, and separating pressure is to carry out under the condition of 8Mpa.
3. the method for claim 1 is characterized in that, also is included in separation temperature and is 35～55 ℃, separating pressure and be under the condition of 4～6Mpa to carry out secondary separation.
4. method as claimed in claim 3 is characterized in that, said secondary separation is 35 ℃ in separation temperature, and separating pressure is to carry out under the condition of 4Mpa.
5. the method for claim 1 is characterized in that, said supercritical CO
2Flow rate of fluid is 25kg/h.
6. the method for claim 1 is characterized in that, the said extraction time is 3～5h.
7. the method for claim 1 is characterized in that, also comprises the step of drying and crushing silkworm chrysalis before the extraction.
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| CN105219521A (en) * | 2015-09-28 | 2016-01-06 | 山东鑫源实业集团有限公司 | A kind of preparation method of silkworm chrysalis oil |
| CN108094551A (en) * | 2017-12-11 | 2018-06-01 | 长春三真实业有限公司 | A kind of silkworm chrysalis oil milk piece that can reduce blood fat |
| CN108157970A (en) * | 2018-02-10 | 2018-06-15 | 海盐县凌特生物科技有限公司 | The preparation method of the compound grease microcapsule of silkworm chrysalis |
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| CN108157970A (en) * | 2018-02-10 | 2018-06-15 | 海盐县凌特生物科技有限公司 | The preparation method of the compound grease microcapsule of silkworm chrysalis |
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