CN111358004A - Low-temperature airflow suspension pinocembrin seed oil pinolenic acid nanoemulsion composition microcapsule - Google Patents
Low-temperature airflow suspension pinocembrin seed oil pinolenic acid nanoemulsion composition microcapsule Download PDFInfo
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- CN111358004A CN111358004A CN201910873440.0A CN201910873440A CN111358004A CN 111358004 A CN111358004 A CN 111358004A CN 201910873440 A CN201910873440 A CN 201910873440A CN 111358004 A CN111358004 A CN 111358004A
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- seed oil
- pinolenic acid
- nanoemulsion composition
- pine seed
- oil
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/115—Fatty acids or derivatives thereof; Fats or oils
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- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/03—Organic compounds
- A23L29/035—Organic compounds containing oxygen as heteroatom
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- A—HUMAN NECESSITIES
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- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/03—Organic compounds
- A23L29/045—Organic compounds containing nitrogen as heteroatom
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- A—HUMAN NECESSITIES
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- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/30—Encapsulation of particles, e.g. foodstuff additives
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- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Abstract
The invention belongs to the technical field of food processing, and discloses a low-temperature air flow suspension red pine seed oil pinolenic acid nanoemulsion composition microcapsule, which is prepared by microencapsulating pine seed oil pinolenic acid nanoemulsion composition which is easy to be oxidized, taking pinolenic acid and morin as core materials, taking zein as wall materials, and preparing powdered oil by a low-temperature air flow suspension method, wherein the content of pinolenic acid after embedding reaches 90.34 +/-0.53%, so that the stability of the pine seed oil pinolenic acid nanoemulsion composition is effectively protected, the generation of bad flavor is effectively controlled, the quality guarantee period of the pine seed oil pinolenic acid nanoemulsion composition is remarkably prolonged, and the problem that the pine seed oil pinolenic acid nanoemulsion composition is easy to be oxidized is solved. The nano-emulsion composition microcapsule prepared by the invention can be directly added into foods such as meat products, dairy products, fruit and vegetable juice and the like, does not influence the taste of the products, and widens the way for the wide application of the nano-emulsion composition microcapsule in the foods.
Description
Technical Field
The invention belongs to the technical field of food processing, and particularly relates to a low-temperature airflow suspension pinocembrin seed oil pinolenic acid nanoemulsion composition microcapsule.
Background
Currently, the closest prior art: the rana chensinensis oil and red pine seed oil microcapsule powder is prepared by taking protein powder and cyclodextrin as wall materials and taking red pine seed oil and rana chensinensis oil as core materials and performing spray drying.
In the process of preparing the capsule, the selection of which wall material is important is one of the important conditions for obtaining the product with high microencapsulation efficiency and high performance. Commonly used wall materials are proteins, hydrocolloids and carbohydrates. In most of the currently reported researches, carbohydrate and protein are used as composite wall materials for embedding, for example, Liu' an and the like use a soybean protein isolate and maltodextrin compound material as a wall material to prepare an oil tea seed oil microcapsule product, so that the oil tea seed oil microcapsule product has good dissolving property and fluidity, and the research of using zein as the wall material to apply to powder oil is not reported.
Zein is a main storage protein in corn, has unbalanced amino acid composition, unique solubility and molecular structure, can form a transparent, soft and uniform preservative film, and is an ideal natural preservative film material. In addition, the zein has very strong emulsibility, can reduce the interfacial tension of oil and water, forms static electricity or space obstruction among liquid drops, effectively prevents the convergence and combination of fat globules, and can change the thickness and the interfacial viscosity of an effective adsorption layer, so that the emulsion formed by compounding has stability in time and space. Meanwhile, the embedding efficiency of the microcapsules is greatly different according to the embedding method, the processing methods such as a spray freezing method, an air suspension method and the like have high energy consumption and high cost, and the spray drying method can also cause the effect destruction and the volatility of heat-sensitive substances, influence the microcapsule particles to generate adverse effects on the properties of food, and limit the application range of the microcapsules in the food. The low-temperature airflow suspension method can effectively promote the combination of the core material and the wall material and improve the embedding efficiency.
In addition, morin is added into the core material, and is a light yellow pigment extracted from barks of Moraceae plants such as phellinus linteus and mulberry and a plurality of Chinese herbal medicines, is a natural bioactive substance and is widely distributed in the natural world. The traditional Chinese medicines of folium Mori, cortex Mori and Mori fructus are respectively from leaf, root bark and fruit of Morus alba L. Mulberry is a medicinal and edible plant and is used as a medicine in east and west. In China, the entry of mulberry into the medicine can be traced to Shen nong Ben Cao Jing, and the later generations of Ben Cao are recorded. Mulberry and its extract have effects of inhibiting enzyme activity, resisting cancer, resisting bacteria, resisting inflammation, resisting atherosclerosis, reducing blood sugar and resisting stress. Moreover, morin has an anti-oxidation effect and can effectively protect pinolenic acid from being oxidized.
In the extraction of morin, an ultrasonic-assisted extraction mode is adopted, wherein ultrasonic-assisted extraction is based on ultrasonic waves, and elastic mechanical vibration generates a high-speed and strong cavitation effect, so that plant cells are broken due to collapse of cavitation bubbles instantly generated in a solvent, and the dissolution of effective components is promoted. Cavitation bubble collapse creates turbulence, high velocity collisions of internal particles and "movement" of microporous particles, thereby promoting vortex diffusion and internal diffusion. In addition, cavitation at solid-liquid surfaces causes the liquid to flow rapidly through the surface cavities. Cavities in the plant surface cause impact by microjets, leading to surface erosion and particle breakdown. These effects provide a new contact area, further promoting mass transfer. The ultrasonic technology is applied to strengthen the process, so that the extraction rate can be effectively improved, the solvent consumption is reduced, the extraction time is shortened, the cost is saved, and the product quality can be improved.
In summary, the problems of the prior art are as follows:
(1) the research of applying zein as a wall material to the powdered oil is not reported.
(2) The microcapsule embedding efficiency is greatly different according to the embedding method, the processing methods such as a spray freezing method, an air suspension method and the like have high energy consumption and high cost, and the spray drying method can also cause the effect destruction and the volatility of heat-sensitive substances, influence microcapsule particles to generate adverse effects on food properties, and limit the application range of the microcapsules in food.
(3) Less antioxidant protection of the core material during embedding.
(4) In the prior art, the embedding rate does not exceed 90 percent, and the processing technology needs to be optimized.
The difficulty of solving the technical problems is as follows:
compared with core material and wall material researches at home and abroad and alcohol soluble protein related reports, exploration processes and processing conditions are required.
Compared with the research in nearly five years at home and abroad, the processing technology is improved, and the optimal embedding rate is obtained through optimizing parameters through a large number of experiments.
The method is suitable for searching the core composite material, and the pinolenic acid is protected while other components are not damaged.
Large amount of data inquiry and experimental exploration.
The significance of solving the technical problems is as follows:
provides new selection and test reference for the wall material of the powdered oil and fat.
The optimal process for embedding the pinus koraiensis seed oil pinolenic acid nanoemulsion composition microcapsules at present is provided, and the low-temperature airflow suspension method can effectively promote the combination of the core material and the wall material and improve the embedding efficiency.
Morin can inhibit enzyme activity while protecting pinolenic acid from oxidation, and has anticancer, antibacterial, antiinflammatory, antiatherosclerotic, blood glucose reducing and anti-stress effects.
The encapsulation rate of the red pine seed oil pinolenic acid nanoemulsion composition microcapsule is improved, and the encapsulation rate can reach more than 97 percent according to the invention.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a low-temperature airflow suspension Korean pine seed oil pinolenic acid nanoemulsion composition microcapsule.
The invention is realized by the following steps that the low-temperature airflow suspension red pine seed oil pinolenic acid nanoemulsion composition microcapsule is composed of the following raw materials in parts by weight: 42 to 43 parts of a mixed oil core material, 12 to 14 parts of a first emulsifier, 43 to 48 parts of a wall material and 8.5 to 10.5 parts of a second emulsifier.
Further, the mixed oil core material is a pinus koraiensis seed oil pinolenic acid nanoemulsion composition (containing evenly mixed morin).
The emulsifier is one or two of monoglyceride and diglyceride fatty acid ester and sucrose fatty acid ester.
The wall material is a mixture of one or more than two of maltodextrin, pentosan, modified starch, gelatin, Arabic gum, sodium alginate and chitosan in any proportion.
The emulsifier is one or a mixture of more than two of sodium caseinate, modified soybean lecithin, sodium stearoyl lactylate and sodium starch octenyl succinate in any proportion.
Furthermore, the particle size of the nano-emulsion composition is 200-250 um.
Further, the pinus koraiensis seed oil pinolenic acid nanoemulsion composition is prepared from the following raw materials in percentage by mass: 15 to 25 percent of surfactant, 0.2 to 0.3 percent of cosurfactant, 1.5 to 8.5 percent of perilla seed oil, 18 to 27 percent of Korean pine seed oil nanoemulsion composition (the content of pinolenic acid is 90 to 95 percent, the content of morin is 5 to 10 percent), 0.15 to 0.85 percent of grape seed oil, 1.5 to 8.5 percent of coix seed oil, 0.2 to 0.3 percent of evening primrose oil and the balance of distilled water, wherein the sum of the mass percent of the raw materials is 100 percent.
One or a mixture of more of the surfactant propylene glycol, span-80 and ethyl oleate.
One or a mixture of more of the cosurfactant polyethylene glycol 400 and isopropanol.
The invention also aims to provide a preparation method of the low-temperature airflow suspension Korean pine seed oil pinolenic acid nanoemulsion composition microcapsule, which comprises the following steps:
step one, preparing a Korean pine seed oil nanoemulsion composition (with pinolenic acid content of 93.78%): adding distilled water into 1 kg-2 kg of red pine nut kernels according to a material-liquid ratio of 4-6 times, homogenizing, putting into an ultrasonic device, carrying out ultrasonic treatment at 25-30 ℃ for 20-30 minutes at 250 w-400 w, adding 0.5-2.5% of protease and cellulase, uniformly stirring at 50-60 ℃, carrying out enzymolysis for 2.5-3 hours, then carrying out enzyme deactivation at 95 ℃ for 10 minutes, centrifuging at 5000-8000 r/min for 30 minutes, carrying out secondary centrifugation under the same conditions, then freezing at-20 ℃ for 24 hours, and separating supernatant pine nut oil after thawing.
Step two, preparation of morin: selecting mulberry leaves, cleaning, drying, crushing, taking mulberry leaf powder (100 g-200 g) which is crushed and sieved (97-900 mu m ocular lens) to soak in acetone, and placing the obtained sample solution in an ultrasonic cleaner for ultrasonic treatment. Separating the extract at 3000r/min for 5-10 min by a centrifuge, collecting supernatant, filtering and distilling under reduced pressure to obtain morin, and uniformly mixing with pine nut oil.
Step three, preparing mixed liquid with the mass ratio of mixed fatty acid to urea being 1: 1.5 and the mass volume ratio of urea to ethanol being 1: 7, adding the mixed liquid into the pine nut oil obtained in the step two, crystallizing at the crystallization temperature of 0 ℃ for 24 hours, and shearing 3-6 cycles by adopting a program of 10000-30000 r/min at an interval of 1min to obtain the pinocembrin seed oil pinoceanic acid nanoemulsion composition.
Step four, preparing a mixed oil core material: weighing 6-10 parts of surfactant and 1 part of cosurfactant according to the formula proportion, adding 12-14 parts of emulsifier I, and putting the mixture into a high-shear emulsifying machine at the temperature of 16 ℃ for high-speed dispersion for 3-5 minutes at 12000r/min to prepare the mixed oil emulsion.
Step five, preparing wall materials: dissolving a wall material in distilled water at 70-90 ℃ to prepare a saturated aqueous solution, mixing 8.5-10.5 parts of an oil-in-water emulsifier II and the wall material aqueous solution, stirring uniformly, then putting into a shearing tank, mixing 42-43 parts of a prepared core material and 43-48 parts of the wall material, putting into the shearing tank, mixing and shearing for 15min to obtain a stable emulsion.
And step six, homogenizing the emulsion twice, and then drying the emulsion in a low-temperature airflow suspension device with the air inlet temperature of 50 ℃ and the air outlet temperature of 45 ℃, wherein the particle size of the obtained product microcapsule is 200-250 mu m, and the product microcapsule can form nano-emulsion composition colloid suspension in the solution.
Further, in the optimization of the addition amount of morin, the change of the antioxidant active substances after the morin and the pinolenic acid are mixed in different proportions is monitored by adopting nuclear magnetic resonance spectroscopy, so that the optimal morin addition amount is obtained.
Further, in the first step, the Korean pine seed oil is prepared by an ultrasonic wave aqueous enzymatic method.
Further, in the step one, 7-9 mL of distilled water is added for preparing the milk composition.
Further, in the first step, 1kg to 2kg of red pine nuts are taken according to a material-liquid ratio of 4 to 6 times, distilled water is added to the red pine nuts, and the mixture is homogenized, stirred and emulsified at a speed of 1000 to 5000r/min for 15 to 30 min.
Further, in the second step, in the preparation of morin, the technological parameters of the ultrasonic generator are ultrasonic treatment for 30min, wherein the frequency is 20 kHz.
Further, in the second step, in the preparation of morin, a vacuum distillation device is used for carrying out vacuum distillation for 2 hours, wherein the vacuum degree is 0.08MPa, the temperature is 70 ℃.
Further, in the third step, pinolenic acid in the red pine seed oil is extracted by urea embedding, mixed fatty acid and urea are added into the pine seed oil at a ratio of 1: 1.5(w/w), the ratio of urea to ethanol is 1: 7(w/v), the crystallization temperature is 0 ℃, the crystallization time is 24 hours, and the pinolenic acid nano-emulsion composition is obtained by shearing 3-6 cycles by adopting a program of 10000-20000-30000 r/min at an interval of 1 min.
Further, in the fourth step, the surfactant is weighed according to the formula proportion, and the surfactant comprises the following raw materials in percentage by mass: 3.0 to 4.5g of propylene glycol, 8 to 805.2 g of span, and 1.2 to 2.5g of ethyl oleate; the cosurfactant is 0.2-0.5 g of polyethylene glycol and 1.4-3.6 g of isopropanol.
Further, in the sixth step, two homogenization parameters are adopted, wherein the first homogenization pressure is 17.4MPa, the second homogenization pressure is 12.8MPa, and the homogenization temperature is 45 ℃.
Another object of the present invention is to provide a low temperature gas flow suspension red pine seed oil pinolenic acid nanoemulsion composition microcapsule produced by the method.
In summary, the advantages and positive effects of the invention are:
the invention is improved on the basis of compounding the classic wall materials of sodium alginate, chitosan and zein, has low energy consumption, and prepares the nano microcapsule particles through high-shear emulsification. The diameter of the microcapsule particle processed by the method is 10-6-10-8 um, and the microcapsule particle can form colloid when added into liquid food, so that suspension is realized, no precipitation is caused, the food taste is not influenced, the emulsibility is enhanced, the oxidation resistance of pinolenic acid is greatly prolonged, and the requirement of the shelf life of food can be completely met. The zein protected by the invention has the advantages of recognized safety, biodegradability, wide source and the like. The pinus koraiensis pinolenic acid has good antioxidant activity, can interact with zein, regulates the self-assembly behavior of the zein, and improves the stability and the antioxidant activity of the emulsion. The influence of the zein-pinolenic acid nanoemulsion composition microcapsules in the low-temperature airflow suspension red pine seed oil pinolenic acid nanoemulsion composition microcapsules on the emulsion stability provides a new idea for the future development of the pine seed oil pinolenic acid.
According to the invention, the pine nut oil pinolenic acid nanoemulsion composition which is easy to oxidize is microencapsulated, pinolenic acid and morin are taken as core materials, zein is taken as a wall material, and powdered oil is prepared by a low-temperature airflow suspension method, the embedding rate can reach more than 97%, the stability of the pine nut oil pinolenic acid nanoemulsion composition is effectively protected, the generation of bad flavor is effectively controlled, the quality guarantee period of the pine nut oil pinolenic acid nanoemulsion composition is remarkably prolonged, and the problem that the pine nut oil pinolenic acid nanoemulsion composition is easy to oxidize is solved; the nano-emulsion composition microcapsule prepared by the invention can be directly added into foods such as meat products, dairy products, fruit and vegetable juice and the like, does not influence the taste of the products, and widens the way for the wide application of the nano-emulsion composition microcapsule in the foods. The invention protects the pinolenic acid content in pine nuts and simultaneously plays the specific effect of unsaturated fatty acid in pine nuts, and combines the functions of antioxidation, sterilization and anticancer of morin, thereby effectively reducing cholesterol and triglyceride, inhibiting vasoconstriction, eliminating the adverse effect of other unsaturated fatty acid on organisms, converting oil from liquid state to solid state for convenient transportation and storage, and being quantitatively and uniformly added into other foods, thereby widening the application range of the pine nut oil pinolenic acid nanoemulsion composition.
Experiments show that: FIG. 4 is a micrograph of a pine seed meal (SEM100x) showing the hot reflux extraction of organic solvent A; b, Soxhlet extraction; and C, ultrasonic-assisted organic solvent extraction.
Through the improvement of the method, the pore distribution of the cell walls in the graphs A and B is obviously dispersed relatively, the relatively complete cell walls exist among the pores, which shows that the cell walls are not broken, residual grease or other components possibly exist and cannot be completely extracted, and the number and the diameter of the pores of the cell walls of the Korean pine seeds after the ultrasonic-assisted extraction in the graph C (the invention) are obviously higher than those in the graphs A and B.
FIG. 5 is a graph showing the influence of the amount of enzyme added and the reaction time on the content of pinolenic acid in the reaction mixture according to the example of the present invention.
FIG. 6 is a graph showing the influence of the amount of distilled water added and the reaction time on the content of pinolenic acid in examples of the present invention.
FIG. 7 is a graph showing the effect of the reaction temperature and reaction time on the content of pinolenic acid in the reaction system according to the embodiment of the present invention.
FIG. 8 is a diagram of a mass spectrometric detection peak of a purified product provided in an embodiment of the present invention.
In the figure: a is a product purified by a traditional urea embedding method; b is a purified product of papain catalysis esterification combined with a zein low-temperature airflow suspension method.
Drawings
Fig. 1 is a flow chart of a preparation method of a low-temperature airflow suspension Korean pine seed oil pinolenic acid nanoemulsion composition microcapsule provided by an embodiment of the invention.
Fig. 2 is a diagram of a process for preparing low-temperature airflow suspension red pine seed oil pinolenic acid nanoemulsion composition microcapsules provided by an embodiment of the present invention.
FIG. 3 is a Nuclear Magnetic Resonance (NMR) spectrum of the antioxidant active substance change map monitored by mixing morin and pinolenic acid in different proportions according to an embodiment of the present invention.
FIG. 4 is a microstructure diagram (SEM100x) of Korean pine seed meal provided in an example of the present invention.
In the figure: a, an organic solvent hot reflux extraction method; b, Soxhlet extraction; c (invention) ultrasonic assisted organic solvent extraction.
FIG. 5 is a graph showing the influence of the amount of enzyme added and the reaction time on the content of pinolenic acid in the reaction mixture according to the example of the present invention.
FIG. 6 is a graph showing the influence of the amount of distilled water added and the reaction time on the content of pinolenic acid in examples of the present invention.
FIG. 7 is a graph showing the effect of the reaction temperature and reaction time on the content of pinolenic acid in the reaction system according to the embodiment of the present invention.
FIG. 8 is a diagram of a mass spectrometric detection peak of a purified product provided in an embodiment of the present invention.
In the figure: a is a product purified by a traditional urea embedding method; b is a purified product of papain catalysis esterification combined with a zein low-temperature airflow suspension method.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In order to solve the problems in the background art, the invention provides a low-temperature airflow suspension Korean pine seed oil pinolenic acid nanoemulsion composition microcapsule and a preparation method thereof. The invention uses sodium alginate, chitosan and zein as wall materials, and pinus koraiensis seed oil pinolenic acid nanoemulsion composition (containing evenly mixed morin) as core materials, and utilizes the characteristic of large contact area of the surface of suspension to obtain the nanoemulsion composition microcapsule by regulating and controlling a low-temperature airflow suspension technology. The zein can reduce the interfacial tension of oil and water, form static electricity or space obstruction among liquid drops, effectively prevent the convergence and combination of fat balls, and change the thickness and interfacial viscosity of an effective adsorption layer, so that the emulsion formed by compounding has stability in time and space. The zein has unique solubility and molecular structure, good ductility, water retention property and elasticity, and good dissolvability and fluidity, so that the pinus koraiensis seed oil pinolenic acid nanoemulsion group microcapsule has wide application prospect in the fields of daily chemicals, textiles and medicines.
To solve the above problems, the application principle of the present invention will be described in detail below.
The invention provides a low-temperature airflow suspension red pine seed oil pinolenic acid nanoemulsion composition microcapsule, which consists of the following raw materials in parts by weight: 42 to 43 parts of a mixed oil core material, 12 to 14 parts of a first emulsifier, 43 to 48 parts of a wall material and 8.5 to 10.5 parts of a second emulsifier.
The mixed oily core material is a pinus koraiensis seed oil pinolenic acid nanoemulsion composition (containing evenly mixed morin).
In the embodiment of the present invention, the emulsifier is one or both of a monoglyceride and a diglyceride fatty acid ester and a sucrose fatty acid ester.
The wall material is a mixture of one or more than two of maltodextrin, pentosan, modified starch, gelatin, Arabic gum, sodium alginate and chitosan in any proportion.
The emulsifier is one or a mixture of more than two of sodium caseinate, modified soybean lecithin, sodium stearoyl lactylate and sodium starch octenyl succinate in any proportion.
In the embodiment of the invention, the particle size of the nano-emulsion composition is 200-250 um.
In the embodiment of the invention, the pinus koraiensis seed oil pinolenic acid nanoemulsion composition is prepared from the following raw materials in percentage by mass: 15 to 25 percent of surfactant, 0.2 to 0.3 percent of cosurfactant, 1.5 to 8.5 percent of perilla seed oil, 18 to 27 percent of Korean pine seed oil nanoemulsion composition (the content of pinolenic acid is 90 to 95 percent, the content of morin is 5 to 10 percent), 0.15 to 0.85 percent of grape seed oil, 1.5 to 8.5 percent of coix seed oil, 0.2 to 0.3 percent of evening primrose oil and the balance of distilled water, wherein the sum of the mass percent of the raw materials is 100 percent.
One or a mixture of more of the surfactant propylene glycol, span-80 and ethyl oleate.
One or a mixture of more of the cosurfactant polyethylene glycol 400 and isopropanol.
The application of the principles of the present invention will now be further described with reference to the accompanying drawings.
As shown in fig. 1, the preparation method of the low-temperature airflow suspension red pine seed oil pinolenic acid nanoemulsion composition microcapsule provided by the embodiment of the present invention includes:
s101: preparation of Korean pine seed oil nanoemulsion composition (pinolenic acid content 93.78%): adding distilled water into 1 kg-2 kg of Korean pine seed oil according to a material-liquid ratio of 4-6 times, homogenizing, putting into an ultrasonic device, performing ultrasonic treatment at 25-30 ℃ for 20-30 min by 250 w-400 w, adding 0.5-2.5% of cellulase and papain, uniformly stirring at 50-60 ℃, performing enzymolysis for 2.5-3 h, inactivating enzyme at 95 ℃ for 10min, centrifuging at 5000-8000 r/min for 30min, performing secondary centrifugation under the same condition, freezing at-20 ℃ for 24h, and separating supernatant Korean pine seed oil after thawing.
S102: preparation of morin: selecting mulberry leaves, cleaning, drying, crushing, soaking crushed and sieved (97-900 mu m ocular) mulberry leaf powder (100 g-200 g) in acetone, and placing the obtained sample solution in an ultrasonic generator for ultrasonic treatment at the frequency of 20kHz for 30 min. Separating the extract at 3000rpm by a centrifuge for 5-10 min, collecting supernatant, filtering, distilling under reduced pressure (vacuum degree of 0.08MPa, temperature of 70 deg.C, and reduced pressure for 2 hr) to obtain morin, and mixing with Korean pine seed oil.
S103: preparing a mixed solution of mixed fatty acid and urea in a mass ratio of 1: 1.5 and urea and ethanol in a mass volume ratio of 1: 7, adding the mixed solution into the pine nut oil obtained in the step S102, crystallizing at 0 ℃ for 24 hours, and shearing 3-6 cycles by adopting a program of 10000-30000 r/min at an interval of 1min to obtain the pinoceric acid nanoemulsion composition.
S104: preparing a mixed oil core material: weighing 6-10 parts of surfactant and 1 part of cosurfactant according to the formula proportion, adding 12-14 parts of emulsifier I, and putting the mixture into a high-shear emulsifying machine at the temperature of 16 ℃ for high-speed dispersion for 3-5 minutes at 12000r/min to prepare the mixed oil emulsion.
S105: preparing a wall material: dissolving a wall material in distilled water at 70-90 ℃ to prepare a saturated aqueous solution, mixing 8.5-10.5 parts of an oil-in-water emulsifier II and the wall material aqueous solution, stirring uniformly, then putting into a shearing tank, mixing 42-43 parts of a prepared core material and 43-48 parts of the wall material, putting into the shearing tank, mixing and shearing for 15min to obtain a stable emulsion.
S106: and (3) homogenizing the emulsion twice, wherein the first homogenizing pressure is 17.4MPa, the second homogenizing pressure is 12.8MPa, the homogenizing temperature is 45 ℃, then, drying is carried out in a low-temperature airflow suspension device with the air inlet temperature of 50 ℃ and the air outlet temperature of 45 ℃, the particle size of the obtained product microcapsule is 200-250 mu m, and the product microcapsule can form nano-emulsion composition colloidal suspension in the solution.
Fig. 2 is a diagram of a process for preparing low-temperature airflow suspension red pine seed oil pinolenic acid nanoemulsion composition microcapsules provided by an embodiment of the present invention.
The invention is further described with reference to specific examples.
Example 1
The invention takes the pinus koraiensis seed oil pinolenic acid and morin as the core material of the nanoemulsion composition microcapsule, and takes sodium alginate, chitosan and zein as the wall material to prepare the pinus koraiensis seed oil pinolenic acid nanoemulsion composition microcapsule (low-temperature airflow suspension pinus koraiensis seed oil pinolenic acid nanoemulsion composition microcapsule), which specifically comprises the following steps:
(1) preparation of Korean pine seed oil nanoemulsion composition (pinolenic acid content 93.78%): adding distilled water into 1kg of red pine nut kernel according to a ratio of 5 times of the material to the liquid, homogenizing, putting into an ultrasonic device, performing ultrasonic treatment at 25 ℃ for 25min at 300w, adding 1.5% of cellulase and papain, uniformly stirring at 55 ℃, performing enzymolysis for 2.5h, inactivating enzyme at 95 ℃ for 10min, centrifuging at 8000r/min for 30min, performing secondary centrifugation under the same conditions, freezing at-20 ℃ for 24h, thawing, and separating supernatant pine nut oil.
(2) Preparation of morin: selecting mulberry leaves, repeatedly cleaning, drying and crushing, taking mulberry leaf powder (150g) which is crushed and sieved (800 mu m ocular lens) to soak in acetone, and then placing the sample solution in an ultrasonic cleaner to carry out ultrasonic treatment with the frequency of 20kHz and the treatment time of 30 min. Separating the extract with centrifuge at 3000rpm for 10min, collecting supernatant, filtering, distilling under reduced pressure (vacuum degree of 0.08MPa, temperature of 70 deg.C, and reduced pressure for 2 hr), removing solution to obtain morin, and adding into oleum Pini koraiensis.
(3) Adding mixed fatty acid and urea into pine nut oil at a ratio of 1: 1.5(w/w), adding urea and ethanol at a ratio of 1: 7(w/v), crystallizing at 0 ℃, crystallizing for 24 hours, and shearing for 6 cycles by adopting a program of 10000-20000-30000 r/min at an interval of 1min to obtain the pinocenic acid nanoemulsion composition.
(4) Preparing a mixed oil core material: weighing 8 parts of surfactant and 1 part of cosurfactant according to the proportion of the formula, adding 12 parts of emulsifier I, and putting the mixture into a high-shear emulsifying machine at the temperature of 16 ℃ for high-speed dispersion for 5 minutes at 12000r/min to prepare the mixed oil emulsion.
(5) Preparing a wall material: dissolving the wall material in 80 ℃ distilled water to prepare a saturated aqueous solution, then mixing 8.5 parts of the oil-in-water emulsifier II with the wall material aqueous solution, stirring uniformly, then putting into a shearing tank, mixing the prepared 43 parts of core material with 48 parts of wall material, and putting into the shearing tank to mix and shear for 15min to obtain the stable emulsion.
(6) And then homogenizing the emulsion twice (the first homogenizing pressure is 17.4MPa, the second homogenizing pressure is 12.8MPa, and the homogenizing temperature is 45 ℃), then drying in a low-temperature airflow suspension device with the air inlet temperature of 50 ℃ and the air outlet temperature of 45 ℃, wherein the particle size of the obtained product microcapsule is 200um, and the product microcapsule can form nano-emulsion composition colloid suspension in the solution.
Example 2
The invention takes the pinus koraiensis seed oil pinolenic acid and morin as the core material of the nanoemulsion composition microcapsule, and takes sodium alginate, chitosan and zein as the wall material to prepare the pinus koraiensis seed oil pinolenic acid nanoemulsion composition microcapsule (low-temperature airflow suspension pinus koraiensis seed oil pinolenic acid nanoemulsion composition microcapsule).
(1) Preparation of Korean pine seed oil nanoemulsion composition (pinolenic acid content 93.78%): adding distilled water into 1kg of red pine nut kernel according to a ratio of 5 times of the material to the liquid, homogenizing, putting into an ultrasonic device, performing ultrasonic treatment at 30 ℃ for 30min at 350w, adding 2.5% of cellulase and papain, uniformly stirring at 60 ℃, performing enzymolysis for 3h, inactivating enzyme at 95 ℃ for 10min, centrifuging at 8000r/min for 30min, performing secondary centrifugation under the same conditions, freezing at-20 ℃ for 24h, thawing, and separating supernatant pine nut oil.
(2) Preparation of morin: selecting mulberry leaves, repeatedly cleaning, drying and crushing, taking mulberry leaf powder (200g) which is crushed and sieved (900 mu m ocular lens) to soak in acetone, and then placing the sample solution in an ultrasonic cleaner to carry out ultrasonic treatment with the frequency of 20kHz and the treatment time of 30 min. Separating the extract with centrifuge at 3000rpm for 10min, collecting supernatant, filtering, distilling under reduced pressure (vacuum degree of 0.08MPa, temperature of 70 deg.C, and reduced pressure for 2 hr), removing solution to obtain morin, and adding into oleum Pini koraiensis.
(3) Adding mixed fatty acid and urea into pine nut oil at a ratio of 1: 1.5(w/w), adding urea and ethanol at a ratio of 1: 7(w/v), crystallizing at 0 ℃, crystallizing for 24 hours, and shearing for 6 cycles by adopting a program of 10000-20000-30000 r/min at an interval of 1min to obtain the pinocenic acid nanoemulsion composition.
(4) Preparing a mixed oil core material: weighing 10 parts of surfactant and 1 part of cosurfactant according to the proportion of the formula, adding 14 parts of emulsifier I, and putting the mixture into a high-shear emulsifying machine at the temperature of 16 ℃ for high-speed dispersion for 5 minutes at 12000r/min to prepare the mixed oil emulsion.
(5) Preparing a wall material: dissolving the wall material in distilled water of 90 ℃ to prepare saturated aqueous solution, then mixing 10.5 parts of oil-in-water emulsifier II with the wall material aqueous solution, stirring uniformly, then pumping into a shearing tank, mixing the prepared core material 42 parts with the prepared wall material 43 parts, pumping into the shearing tank, mixing and shearing for 20min to obtain stable emulsion.
(6) And then homogenizing the emulsion twice (the first homogenizing pressure is 17.4MPa, the second homogenizing pressure is 12.8MPa, and the homogenizing temperature is 45 ℃), then drying in a low-temperature airflow suspension device with the air inlet temperature of 50 ℃ and the air outlet temperature of 45 ℃, wherein the particle size of the obtained product microcapsule is 200um, and the product microcapsule can form nano-emulsion composition colloid suspension in the solution.
Example 3
The invention takes the pinus koraiensis seed oil pinolenic acid and morin as the core material of the nanoemulsion composition microcapsule, and takes sodium alginate, chitosan and zein as the wall material to prepare the pinus koraiensis seed oil pinolenic acid nanoemulsion composition microcapsule (low-temperature airflow suspension pinus koraiensis seed oil pinolenic acid nanoemulsion composition microcapsule), which specifically comprises the following steps:
(1) preparation of Korean pine seed oil nanoemulsion composition (pinolenic acid content 93.78%): adding distilled water into 1kg of red pine nut kernel according to a ratio of 5 times of the material to the liquid, homogenizing, putting into an ultrasonic device, performing ultrasonic treatment at 27 ℃ for 25min at 350w, adding 1.5% of cellulase and papain, uniformly stirring at 55 ℃, performing enzymolysis for 2.5h, inactivating enzyme at 95 ℃ for 10min, centrifuging at 7000r/min for 30min, performing secondary centrifugation under the same conditions, freezing at-20 ℃ for 24h, thawing, and separating supernatant pine nut oil.
(2) Preparation of morin: selecting folium Mori, repeatedly cleaning, oven drying and pulverizing, collecting folium Mori powder (1508) which is pulverized and sieved (900 μm ocular lens), soaking in acetone, and ultrasonic treating with ultrasonic cleaner at 20kHz for 30 min. Separating the extract with centrifuge at 3000rpm for 8min, collecting supernatant, filtering, distilling under reduced pressure (vacuum degree of 0.08MPa, temperature of 70 deg.C, and reduced pressure for 2 hr), removing solution to obtain morin, and adding into oleum Pini koraiensis.
(3) Adding mixed fatty acid and urea into pine nut oil at a ratio of 1: 1.5(w/w), adding urea and ethanol at a ratio of 1: 7(w/v), crystallizing at 0 ℃, crystallizing for 24 hours, and shearing for 5 cycles by adopting a program of 10000-20000-30000 r/min at an interval of 1min to obtain the pinocenic acid nanoemulsion composition.
(4) Preparing a mixed oil core material: weighing 8 parts of surfactant and 1 part of cosurfactant according to the proportion of the formula, adding 13 parts of emulsifier I, and putting the mixture into a high-shear emulsifying machine for high-speed dispersion for 4 minutes at the temperature of 16 ℃ at 12000r/min to prepare the mixed oil emulsion.
(5) Preparing a wall material: dissolving wall materials in 80 ℃ distilled water to prepare saturated aqueous solution, then mixing 9.5 parts of oil-in-water emulsifier and the wall material aqueous solution, stirring uniformly, then pumping into a shearing tank, mixing prepared 42 parts of core materials with 45 parts of wall materials, pumping into the shearing tank, mixing and shearing for 20min to obtain stable emulsion.
(6) And then homogenizing the emulsion twice (the first homogenizing pressure is 17.4MPa, the second homogenizing pressure is 12.8MPa, and the homogenizing temperature is 45 ℃), then drying in a low-temperature airflow suspension device with the air inlet temperature of 50 ℃ and the air outlet temperature of 45 ℃, wherein the particle size of the obtained product microcapsule is 200um, and the product microcapsule can form nano-emulsion composition colloid suspension in the solution.
The effect of the present invention will be described in detail below in conjunction with Nuclear Magnetic Resonance (NMR) spectroscopy and related experiments.
As shown in fig. 3, Nuclear Magnetic Resonance (NMR) spectroscopy monitored the change in antioxidant activity after different ratios of morin and pinolenic acid were mixed. The optimal mixture ratio is determined by an orthogonal test, sensory evaluation is taken as a main examination factor, and an L9(33) orthogonal test is carried out to determine the optimal compound ratio. The factors and levels are shown in table one.
Table one: level meter for orthogonal test factors
Hydroxyl radical (. OH) is a radical having a strong oxidizing ability, and is extremely important as a method for detecting OH because of its high reactivity, short life and low concentration. Chenguo et al proposed a photometric method for generating color by the reaction of morin with hydroxyl radicals. Color measurement of Co + + H by Oxidation of morin2O2The method for generating hydroxyl radical (. OH) by system proposes Co + + H2O2Morin was analyzed for the new system and used for the determination of hydroxyl radical (. OH). The method is used for Co2+ and H2O2The reaction is similar to Fenton reagent to generate hydroxyl radical (. OH), the generated hydroxyl radical reacts with morin to reduce the absorbance, and the generated hydroxyl radical can be indirectly measured by utilizing the change of the absorbance value, so that the optimal experimental condition of the system is determined. Simultaneous determination of antioxidant scavenging hydroxyl radicalsThe experiment of the gene group, combined with ORAC analysis, proves that the system can be used as one of the methods for screening the antioxidant. Table 2 shows the optimization of the proportions of the components in the low-temperature airflow suspension Korean pine seed oil pinolenic acid nanoemulsion composition microcapsule and the preparation method thereof:
table 2: orthogonal test result analysis table
The results of the range analysis in the table show that the primary and secondary relationship of the influence of each factor on acidity is a ═ C > B, that is, the addition amount of morin is zein and the addition amount of pinolenic acid. From the mean, it can be seen that the optimal level for factor A is A3, the optimal level for B is B3, and the optimal level for C is C2, so the optimal combination is A3C2B 3.
The invention is further described below in connection with specific experiments.
Experiments show that: FIG. 4 is a micrograph of a pine seed meal (SEM100x) showing the hot reflux extraction of organic solvent A; b, Soxhlet extraction; and C, ultrasonic-assisted organic solvent extraction.
Through the improvement of the method, the pore distribution of the cell walls in the graphs A and B is obviously dispersed relatively, the relatively complete cell walls exist among the pores, which shows that the cell walls are not broken, residual grease or other components possibly exist and cannot be completely extracted, and the number and the diameter of the pores of the cell walls of the Korean pine seeds after the ultrasonic-assisted extraction in the graph C (the invention) are obviously higher than those in the graphs A and B.
FIG. 5 is a graph showing the influence of the amount of enzyme added and the reaction time on the content of pinolenic acid in the reaction mixture according to the example of the present invention. In the figure, a represents the response relationship between time and enzyme addition amount, and b represents the optimal value of time and enzyme addition amount.
The effect of the reaction time on the results indirectly reflects the efficiency of the entire esterification reaction, and it can be seen from FIG. 5 that the amount of enzyme added as a catalyst in the esterification reaction has a very significant (P < 0.001) effect on the resulting pinolenic acid content. The reaction rate increases with the increase of the amount of enzyme added until the fixed point maximum value is reached, the effect of the esterification reaction by adding excessive enzyme is reduced, and the transfer selectivity of the enzyme is adversely affected.
FIG. 6 is a graph showing the influence of the amount of distilled water added and the reaction time on the content of pinolenic acid in examples of the present invention. In the figure, a represents the response relation between time and water addition amount, and b represents the optimal value of the time and the water addition amount.
The amount of distilled water added has a certain interaction with the reaction efficiency, and it is judged from the trend of the 3D graph that the increase in the amount of water results in a further increase in the pinolenic acid content up to the fixed-point maximum. In the esterification reaction of dodecanol and fatty acid, water as the catalyst for enzyme is an indispensable part of the reaction system, but excessive water can destroy the esterification reaction system to become hydrolysis and reduce the activity of enzyme
FIG. 7 is a graph showing the effect of the reaction temperature and reaction time on the content of pinolenic acid in the reaction system according to the embodiment of the present invention. In the figure, a represents the time and temperature response relationship; b represents the time and temperature optimum.
The two factors of the temperature of the reaction system and the time required by the whole reaction have strong interactivity in most biochemical reactions, the activity of enzyme is gradually excited along with the rise of the reaction temperature in the reaction of catalyzing and esterifying by the complex enzyme, the esterification efficiency is obviously increased along with the progress of the high-efficiency catalyzing and esterifying reaction, and the reaction efficiency begins to decline after the optimum temperature of the complex enzyme is exceeded, so that the final result is reduced.
Analyzing the regression model by using a response surface optimization analysis method, and calculating the optimal response condition as follows: the enzyme addition amount is 1.5 percent, the reaction temperature is 55.7 ℃, the duration is 2.67 hours, and under the condition, the pinolenic acid content of the first-grade purified product reaches 50.75 percent. In order to facilitate the test operation, the reaction temperature and the reaction time are respectively adjusted to 2.7h and 55 ℃, and meanwhile, in order to further verify the reliability of the extraction method, parallel tests are carried out, and the result shows that the average pinolenic acid content of the purified product after esterification is 50.04%, and the difference with the predicted value of the model is not significant (p is less than 0.01).
FIG. 8 is a diagram of a mass spectrometric detection peak of a purified product provided in an embodiment of the present invention.
In the figure: a is a product purified by a traditional urea embedding method; b is a purified product of papain catalysis esterification combined with a zein low-temperature airflow suspension method.
After 36h of freezing crystallization, carrying out suction filtration to remove crystallization, and recovering an organic solvent to obtain a secondary pinolenic acid purified product, carrying out qualitative and quantitative analysis of a gas chromatography mass spectrum after alkaline methyl esterification, and observing from figures 8a and b, the linoleic acid integral peak in a gas phase peak diagram of a fatty acid sample subjected to catalytic esterification is obviously reduced, the pinolenic acid absorption peak is increased, and compared with a pinocembrine oil fatty acid methyl ester chromatographic peak diagram, the fatty acid types in the esterified secondary purified product are obviously reduced, and the main fatty acid components of linoleic acid and oleic acid in the pinocembrine oil are separated and removed under the esterification and embedding effects.
The results of mass spectrometric detection of the main fatty acid contents of the red pine oil and the purified product are shown in table 3 below, in which it can be seen that the linoleic acid content is reduced from 46.24% to 5.22% after esterification embedding purification, and the content changes significantly (p > 0.01) compared with the content after traditional embedding purification; the content of pinolenic acid is increased to 90.34% after esterification and embedding, and is obviously improved compared with the traditional embedding method (51.42%).
TABLE 3 fatty acid content of the main component of the purified product
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The low-temperature airflow suspension Korean pine seed oil pinolenic acid nanoemulsion composition microcapsule is characterized by comprising, by weight, 42-43 parts of a mixed oil core material, 12-14 parts of a first emulsifier, 43-48 parts of a wall material and 8.5-10.5 parts of a second emulsifier.
2. The low-temperature air-flow suspension red pine seed oil pinolenic acid nanoemulsion composition microcapsule of claim 1, wherein the mixed oil core material is a red pine seed oil pinolenic acid nanoemulsion composition;
the emulsifier is one or two of monoglyceride and diglyceride fatty acid ester and sucrose fatty acid ester;
the wall material is a mixture composed of one or more than two of maltodextrin, pentosan, modified starch, gelatin, Arabic gum, sodium alginate and chitosan in any proportion;
and the second emulsifier is one or a mixture of more than two of sodium caseinate, modified soybean lecithin, sodium stearyl lactate and sodium starch octenyl succinate in any proportion.
3. The low-temperature air-flow suspension Korean pine seed oil pinolenic acid nanoemulsion composition microcapsule as claimed in claim 1, wherein the nanoemulsion composition has a particle size of 200-250 um.
4. The low-temperature airflow suspension Korean pine seed oil pinolenic acid nanoemulsion composition microcapsule as claimed in claim 2, wherein the Korean pine seed oil pinolenic acid nanoemulsion composition comprises 15-25% by mass of surfactant, 0.2-0.3% by mass of co-surfactant, 1.5-8.5% by mass of perilla seed oil, 18-27% by mass of Korean pine seed oil nanoemulsion composition, 0.15-0.85% by mass of grape seed oil, 1.5-8.5% by mass of coix seed oil, 0.2-0.3% by mass of evening primrose oil, and the balance of distilled water;
the Korean pine seed oil nanoemulsion composition consists of 90-95% of pinolenic acid and 5-10% of morin according to the mass ratio;
one or a mixture of more of the surfactant propylene glycol, span-80 and ethyl oleate;
one or a mixture of more of the cosurfactant polyethylene glycol 400 and isopropanol.
5. The method for preparing the low-temperature air-flow suspension red pine seed oil pinolenic acid nanoemulsion composition microcapsule according to claim 1, wherein the method for preparing the low-temperature air-flow suspension red pine seed oil pinolenic acid nanoemulsion composition microcapsule comprises the following steps:
step one, preparing a Korean pine seed oil nanoemulsion composition: adding distilled water into 1 kg-2 kg red pine nut kernels according to a material-liquid ratio of 4-6 times, homogenizing, putting into an ultrasonic device, carrying out ultrasonic treatment at 25-30 ℃ for 20-30 minutes at 250 w-400 w, adding 0.5-2.5% of protease and cellulase, uniformly stirring at 50-60 ℃, carrying out enzymolysis for 2.5-3 hours, then carrying out enzyme deactivation at 95 ℃ for 10 minutes, centrifuging at 5000-8000 r/min for 30 minutes, carrying out secondary centrifugation under the same conditions, then freezing at-20 ℃ for 24 hours, thawing, and separating supernatant pine nut oil,
step two, preparation of morin: selecting mulberry leaves, cleaning, drying, crushing, taking 100 g-200 g of crushed and sieved mulberry leaf powder, soaking in acetone, and placing the obtained sample solution in an ultrasonic cleaner for ultrasonic treatment; separating the extract at 3000r/min for 5-10 min with a centrifuge, collecting supernatant, filtering and distilling under reduced pressure to obtain morin, mixing with oleum Pini koraiensis uniformly,
step three, preparing a mixed liquid with the mass ratio of mixed fatty acid to urea being 1: 1.5 and the mass volume ratio of urea to ethanol being 1: 7, adding the mixed liquid into the pine nut oil obtained in the step two, crystallizing at the crystallization temperature of 0 ℃ for 24 hours, and shearing 3-6 cycles by adopting a program of 10000-20000-30000 r/min at an interval of 1min to obtain the pinolenic acid nanoemulsion composition;
step four, preparing a mixed oil core material: weighing 6-10 parts of surfactant and 1 part of cosurfactant according to a formula ratio, adding 12-14 parts of emulsifier I, and putting the mixture into a high-shear emulsifying machine at the temperature of 16 ℃ for high-speed dispersion for 3-5 minutes at 12000r/min to prepare a mixed oil emulsion;
step five, preparing wall materials: dissolving a wall material in distilled water at 70-90 ℃ to prepare a saturated aqueous solution, mixing 8.5-10.5 parts of an oil-in-water emulsifier II and the wall material aqueous solution, stirring uniformly, then feeding into a shearing tank, mixing 42-43 parts of a prepared core material and 43-48 parts of the wall material, feeding into the shearing tank, mixing and shearing for 15min to obtain a stable emulsion;
and step six, homogenizing the emulsion twice, and then drying the emulsion in a low-temperature airflow suspension device with the air inlet temperature of 50 ℃ and the air outlet temperature of 45 ℃, wherein the particle size of the obtained product microcapsule is 200-250 mu m, and the product microcapsule can form nano-emulsion composition colloid suspension in the solution.
6. The method for preparing the low-temperature airflow suspension Korean pine seed oil pinolenic acid nanoemulsion composition microcapsules as claimed in claim 5, wherein in the optimization of the addition amount of morin, the change of antioxidant activity substances after different proportions of morin and pinolenic acid are mixed is monitored by using nuclear magnetic resonance spectroscopy, so that the optimal addition amount of morin is obtained.
7. The method for preparing the low-temperature airflow suspension red pine seed oil pinolenic acid nanoemulsion composition microcapsule as claimed in claim 5, wherein in the first step, the red pine seed oil is prepared by an ultrasonic aqueous enzymatic method.
8. The method for preparing the low-temperature airflow suspension Korean pine seed oil pinolenic acid nanoemulsion composition microcapsule as claimed in claim 5, wherein in the first step, distilled water is added for preparing the emulsion composition in an amount of 7-9 mL.
9. The method for preparing the low-temperature airflow suspension Korean pine seed oil pinolenic acid nanoemulsion composition microcapsule as claimed in claim 5, wherein in the first step, distilled water is added into 1 kg-2 kg of Korean pine seed kernel according to a material-liquid ratio of 4-6 times, and the stirring and emulsification rate is 1000-5000 r/min and the time is 15-30 min.
10. The method for preparing the low-temperature airflow suspension Korean pine seed oil pinolenic acid nanoemulsion composition microcapsule as claimed in claim 5, wherein in the second step, in the preparation of morin, the process parameters of an ultrasonic generator are set to 20kHz, and ultrasonic treatment is carried out for 30 min; in the preparation of morin, a reduced pressure distillation device is used for carrying out reduced pressure distillation for 2h at the vacuum degree of 0.08MPa and the temperature of 70 ℃;
in the third step, pinolenic acid in the red pine seed oil is extracted by urea embedding, mixed fatty acid and urea are added into the pine seed oil according to the mass ratio of 1: 1.5, urea and ethanol are added according to the mass volume ratio of 1: 7, the crystallization temperature is 0 ℃, the crystallization time is 24 hours, and the pinolenic acid nano-emulsion composition is obtained by shearing 3-6 cycles by adopting a program of 10000-30000 r/min at an interval of 1 min;
in the fourth step, the surfactant is weighed according to the formula proportion, and the surfactant comprises the following raw materials in percentage by mass: 3.0 to 4.5g of propylene glycol, 8 to 805.2 g of span, and 1.2 to 2.5g of ethyl oleate; the cosurfactant is 0.2-0.5 g of polyethylene glycol and 1.4-3.6 g of isopropanol;
in the sixth step, two times of homogenization parameters are adopted, wherein the first time of homogenization pressure is 17.4MPa, the second time of homogenization pressure is 12.8MPa, and the homogenization temperature is 45 ℃.
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