CN103300379A - Method for preparing perilla oil powder through composite condensation microencapsulation - Google Patents
Method for preparing perilla oil powder through composite condensation microencapsulation Download PDFInfo
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Abstract
The invention discloses a method for preparing perilla oil powder through composite condensation microencapsulation, and in particular provides a preparation method of a perilla oil microcapsule which is low in cost and stable in property. The preparation method comprises the following steps of: adding an emulsifying agent into a soy isolated protein solution, and stirring to dissolve the emulsifying agent; adjusting the pH value of the solution to ensure that soy isolated protein has same electric charges with sodium alginate; adding perilla oil into the obtained solution, homogenizing to obtain an emulsion, adding a sodium alginate solution into the emulsion, and uniformly stirring; adjusting the temperature of a system to 40-50 DEG C, and adjusting the pH value to ensure that the soy isolated protein has charges opposite to those of the sodium alginate and then a composite condensation product is formed in the system; diluting and reducing the temperature of the composite condensation product by adding water, putting the composite condensation product into an ice bath, and continuously stirring until the temperature is lower than 10 DEG C to ensure that the composite condensation product is gelatinized; adding glucose or pectin into the system, and curing; and filtering, washing, depositing, and performing freeze-drying to obtain a perilla oil microcapsule product. The perilla oil microcapsule product obtained by the method can be widely applied to the fields of foods, medicines and the like.
Description
Technical field
The present invention relates to food processing technology field, particularly relate to a kind of method that microencapsulation prepares the perilla herb oil powder of condensing again.
Background technology
Perilla herb oil is linolenic main meals sources, and its linolenic acid content is up to 53.6%-64%, is one of natural products of the high linolenic content found up to now, therefore is considered to potential functional lipid.In Asian countries, perilla herb oil is widely used as edible oil and treatment asthma among the people and thirsty good medicine.In the zoopery, be rich in linolenic perilla herb oil and have the physiological function that suppresses atherosclerotic and cancer, can also improve immunity and intellectual level.But because the leukotrienes of high-load has very easily oxidized characteristic in the processing transportation in the perilla herb oil, make its extensive use in the commodity field be restricted.Adopt microcapsules technology embedding perilla herb oil, can suppress the wherein oxidation of polyunsaturated fatty acid, prolong product storage period.
Complex coacervation is one of method for preparing microcapsules.Complex coacervation refers to that two kinds of polyelectrolytes that have an opposite charges take place to interact and forms the complex coacervation thing in the aqueous solution, this complex coacervation thing be deposited on emulsion around, again through gelation, solidify the stable microcapsules of back formation.At present, the compound wall materials that complex coacervation is commonly used is gelatin-gum arabic.Because Arabic gum is relatively more expensive, and quality is less stable also, therefore as wall material embedding perilla herb oil cost height, commercial value is low.Crosslinking agent commonly used in the multiple coacervation process is formaldehyde, glutaraldehyde, because formaldehyde, glutaraldehyde are toxic to human body, has limited the application of this technology in food service industry to a great extent.Patent publication No. is CN200810046897.6, denomination of invention discloses a kind of preparation method of perilla herb oil powder for the patent documentation of " preparation method of perilla herb oil powder and perilla herb oil powder ", adopting protein and polysaccharide in its technical scheme is compound wall materials, and adopts spray drying process that perilla herb oil is carried out embedding.But, because the protein poorly water-soluble especially easily condenses, meet the characteristics of hot and cold mutability near isoelectric point, comparatively strict to the control of experiment condition when preparation perilla herb oil microcapsules, complex process.
Summary of the invention
The objective of the invention is the method at existing preparation perilla herb oil microcapsules, provide that a kind of cost is low, the preparation method of the perilla herb oil microcapsules of stable in properties.
For realizing that the technical scheme that purpose of the present invention adopts is:
A kind ofly condense the method that microencapsulation prepares the perilla herb oil powder again, it is characterized in that, comprise the steps:
(1) in soybean protein isolate solution, adds the emulsifier for mixing dissolving;
(2) the pH value of regulating step (1) gained solution makes soybean protein isolate have the electric charge identical with sodium alginate;
(3) add perilla herb oil in step (2) gained solution, homogeneous obtains emulsion, adds sodium alginate soln again in the above-mentioned emulsion and stirs;
(4) regulating step (3) gained system temperature is to 40-50 ℃, and regulates pH value and make soybean protein isolate and sodium alginate have opposite charges, makes the complex coacervation thing of formation soybean protein isolate and sodium alginate to embed perilla herb oil in the system;
(5) thin up cooling in the system of step (4), and place ice bath to continue to be stirred to below 10 ℃, make the gelation of gained complex coacervation thing;
(6) in the system of step (5), add glucose or pectin, solidify;
(7) filtration washing precipitation, freeze drying obtains the perilla herb oil microcapsule product.
Described emulsifying agent is monoglyceride, Tween 80 or sorbester p17, and the addition of emulsifying agent is the 0.1-0.2% of microcapsules gross mass in the step (1).
The mixing wall material of being made up of soybean protein isolate and sodium alginate and the mass ratio of core are 1:1, mix that the mass ratio of soybean protein isolate and sodium alginate is 3:1-4:1 in the wall material.
The mass percent concentration of described sodium alginate soln is 3-4%; The mass percent concentration of described soybean protein isolate solution is 3-4%.
Step (2) is regulated the pH value of gained solution to 7-9 with 10% sodium hydroxide solution.
Step (4) is regulated the pH value to 3.0-3.5 with 10% acetum.
The addition of glucose or pectin is the 0.8-1.5% of microcapsules gross mass in the step (6).
Add emulsifying agent 65 ℃ of following stirring and dissolving in the soybean protein isolate solution in the step (1).
The condition that step (4) forms the complex coacervation thing is: water bath heat preservation reaction 20min.
Homogeneous stirs 1min with the speed of 1000r/min in the step (3).
Compared with prior art, advantage of the present invention is:
1, preparation method of the present invention adopts soybean protein isolate and sodium alginate composite as compound wall materials, system pH is transferred to below the isoelectric point of soybean protein isolate, this moment the soybean protein isolate positively charged, sodium alginate is electronegative, thereby multiple aggregation takes place, form microcapsules.Avoided near soybean protein isolate easily cohesion isoelectric point, met the characteristics of hot and cold mutability, reduced the production difficulty, technology is simple, and cost is low.And quality is more stable, complex coacervation microencapsulation perilla herb oil is used have great importance in food.
2, to adopt glucose or pectin be curing agent to preparation method of the present invention, the product safety health of gained.And glucose can improve the film forming of soybean protein isolate, improves permeability and the obdurability of the soybean protein isolate layer of embedding perilla herb oil, and the structure that can be kept perfectly in the following process condition has been protected inner core well.And for the application of glucose in field of food provides foundation.
3, preparation method of the present invention adopts freeze-drying to obtain dry microcapsule product, the products obtained therefrom good stability, steady quality, when having avoided spray-drying because of the destruction of high temperature to perilla herb oil active ingredient.
4, preparation method of the present invention adopts soybean protein isolate and sodium alginate composite as compound wall materials, and product cost is low.
5, the present invention adopts soybean protein isolate and sodium alginate composite as compound wall materials, adopt the method for regulating pH to make two kinds of wall materials of oppositely charged in the aqueous solution, take place to interact and form the complex coacervation thing, be that modifying agent replaces glutaraldehyde with glucose, thereby obtain edible perilla herb oil powder, make the perilla herb oil microcapsule product of multiple cohesion preparation can obtain extensive use in fields such as food, medicines.
6, the present invention adopts soybean protein isolate and sodium alginate composite as compound wall materials, at soybean protein isolate with before sodium alginate mixes, the pH value of elder generation's regulator solution is to 7-9, the soybean protein isolate isoelectric point is about 4.1, regulating acidity makes soybean protein isolate and sodium alginate have identical charges, two kinds of wall materials are mixed, cause that owing to electric charge neutralizes mutually the wall material condenses the generation condensed phase from solution when avoiding mixing.
Description of drawings
Figure 1 shows that the accelerated oxidation test of in 65 ℃ of insulating boxs, carrying out grease, the change curve of the microcapsule product of gained embodiment 1 peroxide value in storage.
The microcapsule product that Figure 2 shows that embodiment 1 preparation amplifies 250 times stereoscan photograph.
The microcapsule product that Figure 3 shows that embodiment 2 preparations amplifies 500 times stereoscan photograph.
The microcapsule product that Figure 4 shows that embodiment 2 preparations amplifies 1000 times stereoscan photograph.
The specific embodiment
Below in conjunction with specific embodiment the present invention is described in further detail.
Embodiment 1
(1) is the wall material with soybean protein isolate and sodium alginate, respectively soybean protein isolate and sodium alginate is configured to 4% solution.
(2) in soybean protein isolate solution, add emulsifying agent monoglyceride (addition be microcapsules gross mass 0.1%), 65 ℃ of following stirring and dissolving.
(3) regulate the pH value to 9 of above-mentioned solution with 10% sodium hydroxide solution.
(4) in above-mentioned solution, add perilla herb oil, obtain the emulsion of stable homogeneous with the speed high-speed stirred 1min of 1000r/min.Drip the sodium alginate soln of step (1) gained in the above-mentioned emulsion again and stir.Wherein, perilla herb oil is 1:1 with the mass ratio that mixes the wall material, and the mass ratio of soybean protein isolate and sodium alginate is 4:1 in the wall material.
(5) water-bath regulation system temperature to 40 ℃, and with 10% vinegar acid for adjusting pH value to 3.5, water bath heat preservation reaction 20min forms the complex coacervation thing in the system.
(6) in above-mentioned system, add the water dilution cooling of one times of amount, and place ice bath to continue to be stirred to below 10 ℃, make the gelation of gained complex coacervation thing.
(7) add the glucose of microcapsules gross mass 1% in the above-mentioned system, water-bath is solidified 1h down for 40 ℃.
(8) filtration washing precipitation, 40-50 ℃ and the following freeze drying of vacuum 10Pa obtain the perilla herb oil microcapsule product.
The quality test of the product of present embodiment gained is as follows:
1, the mensuration of microcapsule embedded rate is as follows: take by weighing the 2.000g microcapsule product, with 20mL benzinum vibration washing, filter, repeat 2 times, merging filtrate is put into the measuring cup of accurately weighing, place 60 ℃ of baking oven solvent evaporated, measuring cup is placed to cool off in the drier weigh, can get the surface of microcapsule oil quality.
Take by weighing 2.000g microcapsules sample, grind repeatedly repeatedly, absolute ether is made solvent and is namely got total oil content with Soxhlet extraction process mensuration.
Surface oil determination data: the quality 1.9997g of sample, weighing disk quality 16.5091g, solvent evaporated oven dry back quality 16.5667g.
Surface oil content=(16.5667-16.5091)/1.9997=2.88%
Total oil content data: the quality 1.9903g of sample, weighing disk quality 16.3632g, solvent evaporated oven dry back quality 16.9004g.
Total oil content=(16.9004-16.3632)/1.9903=26.99%
Embedding rate=1-2.8804%/26.9909%=89.33%
By above data as can be seen, the perilla herb oil that the method obtains substantially all is embedded in the microcapsules, embedding is effective, has reduced contacting of perilla herb oil and external environment, has effectively prolonged storage period.
2, the mensuration of microcapsules moisture is as follows: 105 ℃ of constant weight methods, accurately take by weighing perilla herb oil microcapsules m, and in 105 ℃ of baking ovens, dry by the fire 2h, in drier, be cooled to room temperature then, be weighed as m
1, repeating above operation, be 1h drying time, claims that again quality is m
2, both differ and are no more than 0.05g.
m=10.0002g，m
1=9.6681g，m
2=9.6683g
Moisture content/%=[10.0002-(9.6681+9.6683)/2]/10.0002 * 100=3.32
3, the mensuration of microcapsules solubility is as follows: take by weighing the 5g microcapsules and put into the 50mL beaker, with 38mL25-30 ℃ of water, divide for several times sample dissolution, and move in the 50mL centrifuge tube, jump a queue, above-mentioned centrifuge tube is placed centrifuge, centrifugal 10min, supernatant inclines, and clean tube wall with sliver, add 38mL25-30 ℃ of water again, continue centrifugally, supernatant inclines, and clean tube wall with tampon, precipitation is washed in the weighing disk of known weight with low amounts of water, evaporating water on boiling water bath moves in 105 ℃ of baking ovens again and is dried to constant weight earlier.Computing formula is:
In the formula, w is example weight (g); w
1Be weighing disk heavy (g); w
2Be weighing disk+insoluble matter heavy (g); A% is sample moisture content.
W=5.0001g，w
1=16.5090g，w
2=17.9409g，a=3.32
Solubility (%)=1-(17.9409-16.5090)/((1-3.32%) * 5.0001)=70.38%
4, the mensuration of SGF experiment is as follows: accurately get the 10g pepsin and be dissolved in the 500mL water, add 0.1mol/L hydrochloric acid adjust pH to 1.2, adding 2g NaCl is diluted to 1000mL with solution and makes simulated gastric fluid.The 1g microcapsules are placed the triangular flask that fills the 100mL simulated gastric fluid, stir in 37 ℃ of waters bath with thermostatic control, mixing speed≤200r/min, record consoluet time of microcapsule product.
Microcapsules sample complete dissolution time under the SGF condition is 4h, and the character of wall material has determined the tolerance of microcapsule product to environment.It is that the microcapsules that the compound wall materials complex coacervation prepares can dissolve under one's belt that the result shows with soybean protein isolate and sodium alginate.
5, the mensuration of the storage-stable of perilla herb oil microcapsules is as follows: the perilla herb oil microcapsules that embodiment 1 is obtained are layered on the culture dish bottom respectively equably with the perilla herb oil crude oil of embedding not, put into insulating box, in 65 ℃ of accelerated oxidation tests of carrying out grease, survey a peroxide value every 24h, the result as shown in Figure 1.Along with the prolongation of time, the peroxide value of the perilla herb oil crude oil of embedding and perilla herb oil microcapsule product does not all have trend of rising as can be seen from Figure 1, but the table of degree that rises reveals very big otherness.In storage, the peroxide value of crude oil rises rapidly, has produced serious bad oil smell.And the microcapsule product of gained is in storage, and the amplitude that peroxide value rises is less, and grease embedding densification is described, effective, oxidation resistance is strong.This shows, the perilla herb oil microencapsulation is significant for prolonging the perilla herb oil shelf-life.
6, the ESEM of perilla herb oil microcapsules the results are shown in Figure 2, be wall material complex coacervation embedding perilla herb oil with soybean protein isolate and sodium alginate as can be seen, the microcapsules cyst wall of gained is smooth, structure is even compact relatively, does not have tangible fold and defective, and configuration of surface is regular, has good mechanical strength, be conducive to improve barrier propterty, thereby avoid the core perilla herb oil to contact with external environment, anti-oxidation.
Embodiment 2
(1) is the wall material with soybean protein isolate and sodium alginate, respectively soybean protein isolate and sodium alginate is configured to 3% solution.
(2) in soybean protein isolate solution, add emulsifier tween 80(addition be the microcapsules gross mass 0.2%), 65 ℃ of following stirring and dissolving.
(3) regulate the pH value to 7 of above-mentioned solution with 10% sodium hydroxide solution.
(4) in above-mentioned solution, add perilla herb oil, obtain the emulsion of stable homogeneous with the speed high-speed stirred 1min of 1000r/min.Drip sodium alginate soln again in the above-mentioned emulsion and stir.Wherein, perilla herb oil is 1:1 with the mass ratio that mixes the wall material, and the mass ratio of soybean protein isolate and sodium alginate is 3:1 in the wall material.
(5) water-bath regulation system temperature to 50 ℃, and with 10% vinegar acid for adjusting pH value to 3.5, water bath heat preservation reaction 20min forms the complex coacervation thing in the system.
(6) in above-mentioned system, add the water dilution cooling of one times of amount, and place ice bath to continue to be stirred to below 10 ℃, make the gelation of gained complex coacervation thing.
(7) add the pectin of microcapsules gross mass 1% in the above-mentioned system, water-bath is solidified 1h down for 40 ℃.
(8) filtration washing precipitation, 40-50 ℃ and the following freeze drying of vacuum 10Pa obtain the perilla herb oil microcapsule product.
The quality test of the microcapsule product of this example gained such as example 1:
1, the mensuration of microcapsule embedded rate is as follows: take by weighing the 2.000g microcapsule product, with 20mL benzinum vibration washing, filter, repeat 2 times, merging filtrate is put into the measuring cup of accurately weighing, place 60 ℃ of baking oven solvent evaporated, measuring cup is placed to cool off in the drier weigh, can get the surface of microcapsule oil quality.
Take by weighing 2.000g microcapsules sample, grind repeatedly repeatedly, absolute ether is made solvent and is namely got total oil content with Soxhlet extraction process mensuration.
Surface oil determination data: the quality 1.9994g of sample, weighing disk quality 15.9972g, solvent evaporated oven dry back quality 16.1101g.
Surface oil content=(16.1101-15.9972)/1.9994=5.65%
Total oil content data: the quality 1.9989g of sample, weighing disk quality 16.3097g, solvent evaporated oven dry back quality 16.6907g.
Total oil content=(16.6907-16.3097)/1.9989=19.06%
Embedding rate=1-5.65%/19.06%=70.36%
By above data as can be seen, the perilla herb oil major part that the method obtains is embedded in the microcapsules, is exposed to the perilla herb oil of surface of microcapsule seldom, has effectively prolonged storage period.
2, the mensuration of microcapsules moisture is as follows: 105 ℃ of constant weight methods, accurately take by weighing perilla herb oil microcapsules m, and in 105 ℃ of baking ovens, dry by the fire 2h, in drier, be cooled to room temperature then, be weighed as m
1, repeating above operation, be 1h drying time, claims that again quality is m
2, both differ and are no more than 0.05g.
m=9.9986g，m
1=9.6885g，m
2=9.6887g
Moisture content/%=[9.9986-(9.6885+9.6687)/2]/9.9986 * 100=3.10
3, the mensuration of microcapsules solubility is as follows: take by weighing the 5g microcapsules and put into the 50mL beaker, with 38mL25-30 ℃ of water, divide for several times sample dissolution, and move in the 50mL centrifuge tube, jump a queue, above-mentioned centrifuge tube is placed centrifuge, centrifugal 10min, supernatant inclines, and clean tube wall with sliver, add 38mL25-30 ℃ of water again, continue centrifugally, supernatant inclines, and clean tube wall with tampon, precipitation is washed in the weighing disk of known weight with low amounts of water, evaporating water on boiling water bath moves in 105 ℃ of baking ovens again and is dried to constant weight earlier.Computing formula is:
In the formula, w is example weight (g); w
1Be weighing disk heavy (g); w
2Be weighing disk+insoluble matter heavy (g); A% is sample moisture content.
W=5.0003g，w
1=15.9975g，w
2=17.6526g，a=3.10
Solubility (%)=1-(17.6526-15.9975)/((1-3.10%) * 5.0003)=65.84%
4, the mensuration of SGF experiment is as follows: accurately get the 10g pepsin and be dissolved in the 500mL water, add 0.1mol/L hydrochloric acid adjust pH to 1.2, adding 2g NaCl is diluted to 1000mL with solution and makes simulated gastric fluid.The 1g microcapsules are placed the triangular flask that fills the 100mL simulated gastric fluid, stir in 37 ℃ of waters bath with thermostatic control, mixing speed≤200r/min, record consoluet time of microcapsule product.
Microcapsules sample complete dissolution time under the SGF condition is 3.5h-4h, it is that the microcapsules that the compound wall materials complex coacervation prepares can dissolve under one's belt that the result shows with soybean protein isolate and sodium alginate, help digestion, at field of food certain application prospect is arranged.
5, perilla herb oil microcapsules ESEM is seen Fig. 3, Fig. 4, and the gained microcapsule product is multinuclear spheroidal as can be seen, smooth surface, and compact structure is embedded in perilla herb oil in the cyst wall, has well avoided perilla herb oil to contact with external environment, can extend the shelf life.
The above only is preferred embodiment 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 improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. one kind is condensed the method that microencapsulation prepares the perilla herb oil powder again, it is characterized in that, comprises the steps:
(1) in soybean protein isolate solution, adds the emulsifier for mixing dissolving;
(2) the pH value of regulating step (1) gained solution makes soybean protein isolate have the electric charge identical with sodium alginate;
(3) add perilla herb oil in step (2) gained solution, homogeneous obtains emulsion, adds sodium alginate soln again in the above-mentioned emulsion and stirs;
(4) regulating step (3) gained system temperature is to 40-50 ℃, and regulates pH value and make soybean protein isolate and sodium alginate have opposite charges, makes the complex coacervation thing of formation soybean protein isolate and sodium alginate to embed perilla herb oil in the system;
(5) thin up cooling in the system of step (4), and place ice bath to continue to be stirred to below 10 ℃, make the gelation of gained complex coacervation thing;
(6) in the system of step (5), add glucose or pectin, solidify;
(7) filtration washing precipitation, freeze drying obtains the perilla herb oil microcapsule product.
2. according to claim 1ly condense the method that microencapsulation prepares the perilla herb oil powder again, it is characterized in that described emulsifying agent is monoglyceride, Tween 80 or sorbester p17, the addition of emulsifying agent is the 0.1-0.2% of microcapsules gross mass in the step (1).
3. according to claim 1 and 2ly condense the method that microencapsulation prepares the perilla herb oil powder again, it is characterized in that, the mixing wall material of being made up of soybean protein isolate and sodium alginate and the mass ratio of core are 1:1, mix that the mass ratio of soybean protein isolate and sodium alginate is 3:1-4:1 in the wall material.
4. according to claim 3ly condense the method that microencapsulation prepares the perilla herb oil powder again, it is characterized in that the mass percent concentration of described sodium alginate soln is 3-4%; The mass percent concentration of described soybean protein isolate solution is 3-4%.
5. according to claim 3ly condense the method that microencapsulation prepares the perilla herb oil powder again, it is characterized in that step (2) is regulated the pH value of gained solution to 7-9 with 10% sodium hydroxide solution.
6. according to claim 3ly condense the method that microencapsulation prepares the perilla herb oil powder again, it is characterized in that step (4) is regulated the pH value to 3.0-3.5 with 10% acetum.
7. according to claim 3ly condense the method that microencapsulation prepares the perilla herb oil powder again, it is characterized in that the addition of glucose or pectin is the 0.8-1.5% of microcapsules gross mass in the step (6).
8. according to claim 3ly condense the method that microencapsulation prepares the perilla herb oil powder again, it is characterized in that, add emulsifying agent 65 ℃ of following stirring and dissolving in the soybean protein isolate solution in the step (1).
9. according to claim 3ly condense the method that microencapsulation prepares the perilla herb oil powder again, it is characterized in that the condition that step (4) forms the complex coacervation thing is: water bath heat preservation reaction 20min.
10. according to claim 3ly condense the method that microencapsulation prepares the perilla herb oil powder again, it is characterized in that homogeneous stirs 1min with the speed of 1000r/min in the step (3).
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| CN113088395A (en) * | 2021-05-10 | 2021-07-09 | 云南中烟工业有限责任公司 | Wild plum microcapsule for cigarettes and preparation method thereof |
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| CN114568674A (en) * | 2022-02-17 | 2022-06-03 | 江南大学 | Preparation method of high-embedding-rate microcapsules for powdering spice essential oil |
| CN115137046A (en) * | 2022-05-30 | 2022-10-04 | 江南大学 | Method for improving freeze-thaw stability of high-moisture emulsified minced fillet gel and product thereof |
| JP7421024B2 (en) | 2022-05-30 | 2024-01-24 | 江南大学 | Method and product for improving the freezing and thawing stability of high-moisture emulsified surimi gel |
| CN114933939A (en) * | 2022-06-10 | 2022-08-23 | 广东优凯科技有限公司 | Essence microcapsule with biodegradable wall material and application thereof in liquid detergent |
| CN115736221A (en) * | 2022-12-06 | 2023-03-07 | 洽洽食品股份有限公司 | Multilayer microencapsulated nut powder and production process thereof |
| CN115997909A (en) * | 2023-02-15 | 2023-04-25 | 郑州雪麦龙食品香料有限公司 | Preparation method of spice essential oil microcapsule with high fluidity |
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Application publication date: 20130918 |