CN108354000A - Fresh-keeping for fresh agricultural products slow, released microcapsule and preparation method thereof - Google Patents
Fresh-keeping for fresh agricultural products slow, released microcapsule and preparation method thereof Download PDFInfo
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- CN108354000A CN108354000A CN201810352304.2A CN201810352304A CN108354000A CN 108354000 A CN108354000 A CN 108354000A CN 201810352304 A CN201810352304 A CN 201810352304A CN 108354000 A CN108354000 A CN 108354000A
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- essential oil
- microcapsules
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- fresh
- pellet
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 123
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000000341 volatile oil Substances 0.000 claims abstract description 82
- 238000013270 controlled release Methods 0.000 claims abstract description 46
- 239000008188 pellet Substances 0.000 claims abstract description 44
- 239000011162 core material Substances 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 33
- 229920002472 Starch Polymers 0.000 claims abstract description 25
- 239000008107 starch Substances 0.000 claims abstract description 25
- 238000000576 coating method Methods 0.000 claims abstract description 22
- 239000011248 coating agent Substances 0.000 claims abstract description 21
- 239000003921 oil Substances 0.000 claims abstract description 16
- 239000002808 molecular sieve Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 7
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 241000744766 Cymbopogon winterianus Species 0.000 claims abstract description 6
- 239000011148 porous material Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000004088 foaming agent Substances 0.000 claims description 20
- 239000001856 Ethyl cellulose Substances 0.000 claims description 12
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 12
- 229920001249 ethyl cellulose Polymers 0.000 claims description 12
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 11
- 239000004745 nonwoven fabric Substances 0.000 claims description 11
- 150000002429 hydrazines Chemical class 0.000 claims description 8
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 8
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 238000010521 absorption reaction Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000002131 composite material Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 5
- 229960003511 macrogol Drugs 0.000 claims description 5
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 4
- 229960003943 hypromellose Drugs 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 2
- 241000196324 Embryophyta Species 0.000 abstract description 7
- 238000004321 preservation Methods 0.000 abstract description 4
- 239000000843 powder Substances 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 230000003115 biocidal effect Effects 0.000 abstract 1
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 18
- 235000019698 starch Nutrition 0.000 description 14
- 241000209094 Oryza Species 0.000 description 9
- 235000007164 Oryza sativa Nutrition 0.000 description 9
- 239000003814 drug Substances 0.000 description 9
- 235000009566 rice Nutrition 0.000 description 9
- 229940079593 drug Drugs 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 240000008042 Zea mays Species 0.000 description 5
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 5
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 5
- 230000003321 amplification Effects 0.000 description 5
- 239000002775 capsule Substances 0.000 description 5
- 235000005822 corn Nutrition 0.000 description 5
- 238000003199 nucleic acid amplification method Methods 0.000 description 5
- 238000004806 packaging method and process Methods 0.000 description 5
- 241000209140 Triticum Species 0.000 description 4
- 235000021307 Triticum Nutrition 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000000796 flavoring agent Substances 0.000 description 3
- 235000019634 flavors Nutrition 0.000 description 3
- 235000012055 fruits and vegetables Nutrition 0.000 description 3
- 235000013372 meat Nutrition 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 241000233866 Fungi Species 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012263 liquid product Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 230000001953 sensory effect Effects 0.000 description 2
- 238000013268 sustained release Methods 0.000 description 2
- 239000012730 sustained-release form Substances 0.000 description 2
- 240000004784 Cymbopogon citratus Species 0.000 description 1
- 235000017897 Cymbopogon citratus Nutrition 0.000 description 1
- 206010067482 No adverse event Diseases 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003260 anti-sepsis Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000013265 extended release Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- -1 molecular sieve compound Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B4/00—General methods for preserving meat, sausages, fish or fish products
- A23B4/14—Preserving with chemicals not covered by groups A23B4/02 or A23B4/12
- A23B4/18—Preserving with chemicals not covered by groups A23B4/02 or A23B4/12 in the form of liquids or solids
- A23B4/20—Organic compounds; Microorganisms; Enzymes
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B7/00—Preservation or chemical ripening of fruit or vegetables
- A23B7/14—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10
- A23B7/153—Preserving or ripening with chemicals not covered by groups A23B7/08 or A23B7/10 in the form of liquids or solids
- A23B7/154—Organic compounds; Microorganisms; Enzymes
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Microbiology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a kind of fresh-keeping for fresh agricultural products slow, released microcapsules and preparation method thereof, include the release-controlled film microcapsules of 5 kinds of different coating film thicknesses, each release-controlled film microcapsules is made of release-controlled film, pellet essential oil microcapsules, release-controlled film is the water-insoluble release-controlled film that water soluble pore formers are distributed with, and the core material of pellet essential oil microcapsules is porous-starch or micro porous molecular sieve；The core material of pellet essential oil microcapsules is mixture of the edible purity up to 99% or more Herba Origani Vulgaris quintessence oil, galic essential oil and oil of Cymbopogon winterianus.Liquid essential oil is become solid powder by the present invention, it is applied to distributing fresh agricultural products preservation field, effectively controllable release system can be formed, extend the bacteriostasis, preservation time of plants essential oil, and enhancing the stability of essential oil, obtained slow, released microcapsule has preferable biocidal property, safety, stability and zero level controlled release.
Description
Technical field
The invention belongs to Micro-Encapsulation Technique fields, and in particular to a kind of slow, controlled release fresh-keeping for fresh agricultural products
Microcapsules, the invention further relates to the preparation methods of the capsule.
Background technology
Part natural plant essential oils have the characteristics that good anti-bacterial effect, safe and non-toxic, are widely used in food packaging guarantor
Fresh field, however be mostly that plants essential oil is coated on the base materials such as paper, plastic foil, biomembrane or directly sprays essential oil at present
Or the mode of dipping is for the fresh-keeping of fresh agricultural products such as fruits and vegetables or fresh meat.Since plants essential oil stability is poor, process is being used
In be easy to run off；And evaporation rate is uncontrollable, concentration is too small to be not enough to inhibit the growth of microorganism, it is excessive then may to fruits and vegetables or
Fresh meat, which generates, poisons or introduces peculiar smell；Simultaneously essential oil and fresh agricultural products be partly or entirely in direct contact can to the color of food,
The sensory properties such as flavor impact, and reduce the desire to purchase of consumer, to affect its application as antisepsis antistaling agent.
Invention content
The object of the present invention is to provide a kind of slow, released microcapsules fresh-keeping for fresh agricultural products, solve liquid plant
Object essential oil is to fresh product fungi, bacteria suppression effect difference and is in direct contact and can be made to sensory properties such as color, the flavors of food
The problem of at influencing.
The present invention also provides a kind of slow, released microcapsule preparation methods fresh-keeping for fresh agricultural products.
The technical solution adopted in the present invention is, the slow, released microcapsule fresh-keeping for fresh agricultural products, including 5 kinds not
With the release-controlled film microcapsules of coating film thickness, each release-controlled film microcapsules is made of release-controlled film, pellet essential oil microcapsules, controlled release
Film is the water-insoluble release-controlled film that water soluble pore formers are distributed with, and the wall material of pellet essential oil microcapsules is porous-starch or micropore point
Son sieve；The core material of pellet essential oil microcapsules is that edible purity is smart up to 99% or more Herba Origani Vulgaris quintessence oil, galic essential oil and lemongrass
The mixture of oil.
The features of the present invention also characterized in that
Release-controlled film is made of as the ethyl alcohol of water-insoluble base material, 95% as solvent and pore-foaming agent ethyl cellulose EC；
Pore-foaming agent is one kind in Macrogol 6000 and hypromellose HPMC.
The core wall ratio of pellet essential oil microcapsules is 0.3-0.5:1mL/g.
The ratio of water-insoluble base material, solvent and pore-foaming agent is 4:100:1(g/mL/g).
5 kinds of different pellet essential oil microcapsules of release-controlled film microcapsules for being coated film thicknesses and the ratio of release-controlled film are respectively 5:0、
5:5、5:6、5:7、5:8(g/mL)。
The quality proportioning of the release-controlled film microcapsules of 5 kinds of different coating thicknesses is 5:1:1:1:1.
The volume ratio of Herba Origani Vulgaris quintessence oil, galic essential oil and oil of Cymbopogon winterianus is 5 in mixture:2:8.
The another technical solution of the present invention, slow, released microcapsule the preparation method fresh-keeping for fresh agricultural products, tool
Body follows the steps below:
Step 1, the preparation of pellet essential oil microcapsules
In the pellet wall material merging container for weighing certain mass, by core wall ratio 0.3-0.5:Core material is added in the ratio of 1mL/g,
50-70min is shaken in gas bath constant temperature oscillator, makes the fully dispersed absorption composite essential oil of pellet wall material, it is uniform to obtain form
Pellet essential oil microcapsules；
Step 2, the preparation of controlled release film liquid
It is 4 to take mixed proportion:100:The ethyl cellulose EC of 1 (g/mL/g), 95% ethyl alcohol, pore-foaming agent, with digital display top
It sets formula electronic stirrer and stirs 2-4h under the conditions of 15-20 DEG C, 700-900r/min and obtain uniformly mixed controlled release film liquid；
Step 3, delay, the preparation of released microcapsule
The pellet essential oil microcapsules for taking 5 parts of steps 1 to prepare, by the mass body of 5 parts of pellet essential oil microcapsules and controlled release film liquid
Product is than being respectively 5:0、5:5、5:6、5:7、5:8 (g/mL) spray controlled release film liquid respectively to 5 parts of pellet essential oil microcapsules, with true
Vacuum freecing-dry machine freezes 3-8h in -50 DEG C of cold hydrazines, and is dried in vacuo 8-16h under less than 10Pa vacuum degrees and obtains 5 kinds not
With the release-controlled film microcapsules of coating thickness, and in mass ratio 5:1:1:1:1 ratio uniform mixing, is used in combination non-woven fabrics to be packaged into small
Unit to get.
Gas bath constant temperature oscillator is shaken in the 20-25 DEG C of speed with 150-300r/min in step 1.
The invention has the advantages that slow, released microcapsule can embed plants essential oil, improvement can be played and be wrapped by core
The physical properties such as color, appearance, the dissolubility of material；The stability for improving core material, keeps core material not protected from environmental, reduces core material
To the adverse effect of environment；Shield core material smell；Prevent the volatilization of core material active ingredient；Make core material that there is sustained release or controlled capability
Matter；Liquid essential oil is become into solid powder etc..It is applied to distributing fresh agricultural products preservation field, effective can control can be formed and released
Place system, extends the bacteriostasis, preservation time of plants essential oil, and enhances the stability of essential oil.
Description of the drawings
Fig. 1 is the SEM shape appearance figures for 10000 times of the release-controlled film microcapsules amplification that 0ml coating solutions are added in the present invention according to the ratio；
Fig. 2 is the SEM shape appearance figures for 10000 times of the release-controlled film microcapsules amplification that 5ml coating solutions are added in the present invention according to the ratio；
Fig. 3 is the SEM shape appearance figures for 10000 times of the release-controlled film microcapsules amplification that 6ml coating solutions are added in the present invention according to the ratio；
Fig. 4 is the SEM shape appearance figures for 10000 times of the release-controlled film microcapsules amplification that 7ml coating solutions are added in the present invention according to the ratio；
Fig. 5 is the SEM shape appearance figures for 10000 times of the release-controlled film microcapsules amplification that 0ml coating solutions are added in the present invention according to the ratio；
Fig. 6 is slow, released microcapsule the shape appearance figure obtained after the present invention mixes；
Fig. 7 is the packaging unit that the present invention delays, released microcapsule is made with non-woven fabrics；
Fig. 8 is the cumulative release rate diagram of the slow of the embodiment of the present invention 1, released microcapsule core material；
Fig. 9 is the cumulative release rate diagram of the slow of the embodiment of the present invention 2, released microcapsule core material.
Specific implementation mode
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
The present invention slow, released microcapsule fresh-keeping for fresh agricultural products, includes the release-controlled film of 5 kinds of different coating film thicknesses
Microcapsules, each release-controlled film microcapsules are made of release-controlled film, pellet essential oil microcapsules, and release-controlled film is that water-soluble pore is distributed with
The wall material of the water-insoluble release-controlled film of agent, pellet essential oil microcapsules is porous-starch or micro porous molecular sieve；Pellet essential oil microcapsules
Core material be edible purity up to 99% or more Herba Origani Vulgaris quintessence oil, galic essential oil and oil of Cymbopogon winterianus mixture.
The features of the present invention also characterized in that
Release-controlled film is made of as the ethyl alcohol of water-insoluble base material, 95% as solvent and pore-foaming agent ethyl cellulose EC；
Pore-foaming agent is one kind in Macrogol 6000 and hypromellose HPMC.
The core wall ratio of pellet essential oil microcapsules is 0.3-0.5:1mL/g.
The ratio of water-insoluble base material, solvent and pore-foaming agent is 4:100:1(g/mL/g).
5 kinds of different pellet essential oil microcapsules of release-controlled film microcapsules for being coated film thicknesses and the ratio of release-controlled film are respectively 5:0、
5:5、5:6、5:7、5:8(g/mL)。
The quality proportioning of the release-controlled film microcapsules of 5 kinds of different coating thicknesses is 5:1:1:1:1.
The volume ratio of Herba Origani Vulgaris quintessence oil, galic essential oil and oil of Cymbopogon winterianus is 5 in mixture:2:8.
The another technical solution of the present invention, slow, released microcapsule the preparation method fresh-keeping for fresh agricultural products, tool
Body follows the steps below:
Step 1, the preparation of pellet essential oil microcapsules
In the pellet wall material merging container for weighing certain mass, by core wall ratio 0.3-0.5:Core material is added in the ratio of 1mL/g,
50-70min is shaken in gas bath constant temperature oscillator, makes the fully dispersed absorption composite essential oil of pellet wall material, it is uniform to obtain form
Pellet essential oil microcapsules；
Step 2, the preparation of controlled release film liquid
It is 4 to take mixed proportion:100:The ethyl cellulose EC of 1 (g/mL/g), 95% ethyl alcohol, pore-foaming agent, with digital display top
It sets formula electronic stirrer and stirs 2-4h under the conditions of 15-20 DEG C, 700-900r/min and obtain uniformly mixed controlled release film liquid；
Step 3, delay, the preparation of released microcapsule
The pellet essential oil microcapsules for taking 5 parts of steps 1 to prepare, by the mass body of 5 parts of pellet essential oil microcapsules and controlled release film liquid
Product is than being respectively 5:0、5:5、5:6、5:7、5:8 (g/mL) spray controlled release film liquid respectively to 5 parts of pellet essential oil microcapsules, with true
Vacuum freecing-dry machine freezes 3-8h in -50 DEG C of cold hydrazines, and is dried in vacuo 8-16h under less than 10Pa vacuum degrees and obtains 5 kinds not
With the release-controlled film microcapsules of coating thickness, and in mass ratio 5:1:1:1:1 ratio uniform mixing, is used in combination non-woven fabrics to be packaged into small
Unit to get.
Gas bath constant temperature oscillator is shaken in the 20-25 DEG C of speed with 150-300r/min in step 1.
It, can be by several non-woven fabrics packaging units as the barrier preferable polybag of steam when the capsule of the present invention is not used
In, avoid the release of core material；In use, by non-woven fabrics packaging unit as loading in fresh agricultural products rack, due to slow, controlled release
The contact with moisture that microcapsules are carried or volatilized with fresh agricultural products leads to the dissolving of water soluble pore formers, to release essential oil gas
Body plays fresh-keeping effect.
The essential oil of liquid is become solid-state and used by the present invention, enhances the stability of core material, use is more convenient；The core
Material has good inhibition to the common rot-causing fungi of fresh agricultural products, bacterium, and has good smell；Essential oil can be achieved
Sustained release and controlled release simultaneously avoid being in direct contact with fresh agricultural products, influence of the reduction essential oil to fresh agricultural products flavor and color and luster.
Wall material used, core material, release-controlled film are all the material of grade-safe, are had no adverse effects to food；Controlled release processing is not over drawing
Entering to change PH, charge and larger temperature difference etc. can be with the conventional outside inducement of controlled release Release of core material, merely with fruits and vegetables and fresh meat
The release of this factor controlling released microcapsule core material of the larger feature of the humidity of the two, processing procedure are simple.It is released several
The different pellet essential oil microcapsules of medicine rate are combined in different ratios, can easily be adjusted the drug release rate of core material drug, be made
Used time can both make spatial concentration be rapidly reached effective concentration, can avoid the lag time problem of general spansule, and can maintain
Longer action time keeps drug release concentration curve steady, changes simultaneously the pellet ratio of different rate of releasing drug, you can is suitable for more
The fresh-keeping packaging of kind agricultural product.The grain size of porous-starch is located in certain range, has more fixed surface area, and sphere has
There are preferable compressive effect, drug release area relative constant；The drug release behavior of released microcapsule is one unit part of composition simultaneously
The released microcapsule of the summation of each coating microcapsules particle drug release behavior, usual unit part is micro- by thousands of coatings
Capsule particle forms, and individual errors or defect for being coated microcapsules particle in preparation will not generate whole release behavior tight
Ghost image is rung, therefore preparation process is simple and has good reproducibility and consistency in release rule.
Embodiment 1
The preparation of step 1 wheat porous-starch essential oil microcapsules
In the wheat porous-starch merging container for weighing certain mass, by core wall than 0.4:Core is added in the ratio of 1 (mL/g)
Material, in gas bath constant temperature oscillator, 25 DEG C of speed with 200r/min shakes 60min, makes the fully dispersed absorption composite precision of pellet
Oil obtains the uniform wheat porous-starch essential oil microcapsules of form；
The preparation of step 2 controlled release film liquid
4g ethyl cellulose EC are taken, the ethyl alcohol of 100mL95% is injected, and 1g pore-foaming agent Macrogol 6000s are added, use number
Aobvious overhead type electronic stirrer stirs 2h at 20 DEG C, under the conditions of 800r/min and obtains uniformly mixed controlled release film liquid；
Step 3 is slow, released microcapsule preparation
Take 5 parts of steps 1 prepare wheat porous-starch essential oil microcapsules, every part is 5g, respectively uniformly sprinkling 0,5,6,
7, the controlled release film liquid of 8mL freezes 4h, and the vacuum under less than 10Pa vacuum degrees with vacuum freeze drier in -50 DEG C of cold hydrazines
Dry 12h obtains the release-controlled film microcapsules of 5 kinds of different coating thicknesses, and in mass ratio 5:1:1:1:1 ratio uniform mixing, and
Junior unit is packaged into get such as attached drawing 7 with non-woven fabrics.By the SEM shape appearance figures after the coating solution of different ml are added in attached drawing 1-5
Then release-controlled film thickens for the increase for illustrating with controlled release film liquid dosage, and permeability duct quantity is caused to reduce；Attached drawing 8 is demonstrated not
Microcapsules with rate of release are put together with certain proportioning, so that it may achieve the effect that controlled release for a long time.
Embodiment 2
The preparation of step 1 rice porous starch essential oil microcapsules
In the rice porous starch merging container for weighing certain mass, by core wall than 0.4:Core is added in the ratio of 1 (mL/g)
Material, in gas bath constant temperature oscillator, 23 DEG C of speed with 150r/min shakes 50min, makes the fully dispersed absorption composite precision of pellet
Oil obtains the uniform rice porous starch essential oil microcapsules of form；
The preparation of step 2 controlled release film liquid
3.6g ethyl cellulose EC are taken, the ethyl alcohol of 90mL95% is injected, and 0.9g pore-foaming agent hypromellose is added,
2h, which is stirred, with digital display overhead type electronic stirrer at 15 DEG C, under the conditions of 700r/min obtains uniformly mixed controlled release film liquid；
Step 3 is slow, released microcapsule preparation
Take 5 parts of steps 1 prepare rice porous starch essential oil microcapsules, every part is 10g, respectively uniformly sprinkling 0,10,
12, the controlled release film liquid of 14,16mL freezes 3h with vacuum freeze drier in -50 DEG C of cold hydrazines, and under less than 10Pa vacuum degrees
Vacuum drying 8h obtains the release-controlled film microcapsules of 5 kinds of different coating thicknesses, and in mass ratio 5:1:1:1:1 ratio uniform is mixed
Close, be used in combination non-woven fabrics be packaged into junior unit to get.Attached drawing 9, which demonstrates released microcapsule manufactured in the present embodiment and can reach, to be continued
The effect of long-time controlled release
Embodiment 3
The preparation of step 1 rice porous starch essential oil microcapsules
In the rice porous starch merging container for weighing certain mass, by core wall than 0.5:Core material is added in the ratio of 1mL/g,
In gas bath constant temperature oscillator, 20 DEG C of speed with 300r/min shakes 70min, makes rice porous starch is fully dispersed to absorb again
Essential oil is closed, the uniform rice porous starch essential oil microcapsules of form are obtained；
The preparation of step 2 controlled release film liquid
4.4g ethyl cellulose EC are taken, the ethyl alcohol of 110mL95% is injected, and 1.1g pore-foaming agent hydroxypropyl methylcelluloses are added
Element stirs 4h with digital display overhead type electronic stirrer at 17 DEG C, under the conditions of 900r/min and obtains uniformly mixed controlled release film liquid；
Step 3 is slow, released microcapsule preparation
Take 5 parts of steps 1 prepare rice porous starch essential oil microcapsules, every part is 5g, respectively uniformly sprinkling 0,5,6,
7, the controlled release film liquid of 8mL freezes 5h, and the vacuum under less than 10Pa vacuum degrees with vacuum freeze drier in -50 DEG C of cold hydrazines
Dry 16h obtains the release-controlled film microcapsules of 5 kinds of different coating thicknesses, and in mass ratio 5:1:1:1:1 ratio uniform mixing, and
With non-woven fabrics be packaged into junior unit to get.
Embodiment 4
The preparation of step 1 micro porous molecular sieve essential oil microcapsules
In the micro porous molecular sieve merging container for weighing certain mass, by core wall than 0.35:Core material is added in the ratio of 1mL/g,
In gas bath constant temperature oscillator, 22 DEG C of speed with 250r/min shakes 55min, keeps the fully dispersed absorption of micro porous molecular sieve compound
Essential oil obtains the uniform micro porous molecular sieve essential oil microcapsules of form；
The preparation of step 2 controlled release film liquid
3.8g ethyl cellulose EC are taken, the ethyl alcohol of 95mL95% is injected, and 0.95g pore-foaming agent hydroxypropyl methylcelluloses are added
Element stirs 2.5h with digital display overhead type electronic stirrer at 17 DEG C, under the conditions of 750r/min and obtains uniformly mixed controlled release film liquid；
Step 3 is slow, released microcapsule preparation
Take 5 parts of steps 1 prepare micro porous molecular sieve essential oil microcapsules, every part is 10g, respectively uniformly sprinkling 0,10,12,
14, the controlled release film liquid of 16mL freezes 4h with vacuum freeze drier in -50 DEG C of cold hydrazines, and true under less than 10Pa vacuum degrees
The dry 10h of sky obtains the release-controlled film microcapsules of 5 kinds of different coating thicknesses, and in mass ratio 5:1:1:1:1 ratio uniform mixing,
Be used in combination non-woven fabrics be packaged into junior unit to get.
Embodiment 5
The preparation of step 1 corn porous starch essential oil microcapsules
In the corn porous starch merging container for weighing certain mass, by core wall than 0.45:Core is added in the ratio of 1mL/g
Material, in gas bath constant temperature oscillator, 24 DEG C of speed with 250r/min shakes 65min, makes the fully dispersed suction of corn porous starch
Composite essential oil is received, the uniform corn porous starch essential oil microcapsules of form are obtained；
The preparation of step 2 controlled release film liquid
4.2g ethyl cellulose EC are taken, the ethyl alcohol of 105mL95% is injected, and 1.05g pore-foaming agent Macrogol 6000s are added,
3.5h, which is stirred, with digital display overhead type electronic stirrer at 17 DEG C, under the conditions of 850r/min obtains uniformly mixed controlled release film liquid；
Step 3 is slow, released microcapsule preparation
Take 5 parts of steps 1 to prepare corn porous starch essential oil microcapsules, every part is 5g, respectively uniformly sprinkling 0,5,6,7,
The controlled release film liquid of 8mL freezes 7h with vacuum freeze drier in -50 DEG C of cold hydrazines, and vacuum is dry under less than 10Pa vacuum degrees
Dry 14h obtains the release-controlled film microcapsules of 5 kinds of different coating thicknesses, and in mass ratio 5:1:1:1:1 ratio uniform mixing, is used in combination
Non-woven fabrics be packaged into junior unit to get.
The principle of the present invention is：Pellet such as porous-starch has large specific surface area and a large amount of cellular holes, can will be with
Its essential oil mixed fully adsorbs, then by the porous-starch microcapsules controlled release film coating after absorption essential oil, controlled release film thickness
Difference, can be obtained the microcapsules of different rates of release, and the controlled release film thickness of capsule depends on the dosage of controlled release film liquid, controlled release film liquid
The more big then release-controlled film of dosage is thicker, and film is thicker, and permeability duct effective aperture becomes smaller, and effective channel complications are elongated, then microcapsules
Release of core material rate is slower and steady；Using insoluble polymer ethyl cellulose as controlled release film base material, and in release-controlled film
Water soluble pore formers are added in liquid, pore-foaming agent is in an environment with high humidity or chance water is slowly dissolved or fallen off, the shape in clothing film
At many micropores, with the increase of controlled release film thickness, pore-foaming agent layer distributed straggly, under super-humid conditions, the dissolving of upper layer pore-foaming agent
Afterwards, the possibility or base material of lower layer's distribution, still without effective channel；Therefore it utilizes and is caused in controlled release film thickness difference and clothing film
The content of hole agent adjusts the rate of releasing drug of pellet essential oil microcapsules, is the extended release time, can be by several batches of claddings of microcapsules point
The release-controlled film of different-thickness, or reserve a batch and do not do cladding processing as quick-release microcapsules, then the micro- of different rates of release
Capsule is put together with certain proportioning, so that it may achieve the effect that controlled release for a long time.
Claims (9)
1. the slow, released microcapsule fresh-keeping for fresh agricultural products, which is characterized in that include the control of 5 kinds of different coating film thicknesses
Film microcapsules are released, each described release-controlled film microcapsules is made of release-controlled film, pellet essential oil microcapsules, and the release-controlled film is distribution
It is porous-starch or micro porous molecular sieve to have the water-insoluble release-controlled film of water soluble pore formers, the pellet essential oil microcapsules wall material；
The core material of the pellet essential oil microcapsules is Herba Origani Vulgaris quintessence oil, galic essential oil and oil of Cymbopogon winterianus of the edible purity up to 99% or more
Mixture.
2. the slow, released microcapsule fresh-keeping for fresh agricultural products according to claim 1, which is characterized in that the control
Film is released to be made of as solvent and pore-foaming agent as the ethyl alcohol of water-insoluble base material, 95% ethyl cellulose EC；The pore-foaming agent
For one kind in Macrogol 6000 and hypromellose.
3. the slow, released microcapsule fresh-keeping for fresh agricultural products according to claim 1, which is characterized in that described micro-
The core wall ratio of ball essential oil microcapsules is (0.3-0.5)：1ml/g.
4. the slow, released microcapsule fresh-keeping for fresh agricultural products according to claim 2, which is characterized in that the water
The ratio of insoluble base material, solvent and pore-foaming agent is 4:100:1(g/mL/g).
5. the slow, released microcapsule fresh-keeping for fresh agricultural products according to claim 1, which is characterized in that 5 kinds of differences
The pellet essential oil microcapsules of the release-controlled film microcapsules and the mass volume ratio of release-controlled film for being coated film thickness are respectively 5:0、5:
5、5:6、5:7、5:8(g/mL)。
6. the slow, released microcapsule fresh-keeping for fresh agricultural products according to claim 1, which is characterized in that described 5 kinds
The quality proportioning of the release-controlled film microcapsules of different coating thicknesses is 5:1:1:1:1.
7. the slow, released microcapsule fresh-keeping for fresh agricultural products according to claim 1, which is characterized in that described mixed
The volume ratio for closing Herba Origani Vulgaris quintessence oil, galic essential oil and oil of Cymbopogon winterianus in object is 5:2:8.
8. such as slow, released microcapsule the preparation side fresh-keeping for fresh agricultural products according to any one of claims 1 to 7
Method, which is characterized in that specifically include following steps：
Step 1, the preparation of pellet essential oil microcapsules
In the pellet wall material merging container for weighing certain mass, by core wall ratio 0.3-0.5:Core material is added in the ratio of 1mL/g, in gas
50-70min is shaken in bath constant temperature oscillator, makes the fully dispersed absorption composite essential oil of pellet wall material, obtains the uniform pellet of form
Essential oil microcapsules；
Step 2, the preparation of controlled release film liquid
It is 4 to take mixed proportion:100:The ethyl cellulose EC of 1 (g/mL/g), 95% ethyl alcohol, pore-foaming agent, with digital display overhead type
Electronic stirrer stirs 2-4h under the conditions of 15-20 DEG C, 700-900r/min and obtains uniformly mixed controlled release film liquid；
Step 3, delay, the preparation of released microcapsule
The pellet essential oil microcapsules for taking 5 parts of steps 1 to prepare, by the mass volume ratio of 5 parts of pellet essential oil microcapsules and controlled release film liquid
Respectively 5:0、5:5、5:6、5:7、5:8 (g/mL) spray controlled release film liquid respectively to 5 parts of pellet essential oil microcapsules, cold with vacuum
Lyophilizer freezes 3-8h in -50 DEG C of cold hydrazines, and is dried in vacuo 8-16h under less than 10Pa vacuum degrees and obtains 5 kinds of different packets
The release-controlled film microcapsules of clothing thickness, and in mass ratio 5:1:1:1:1 ratio uniform mixing, is used in combination non-woven fabrics to be packaged into small list
Member to get.
9. slow, released microcapsule the preparation method fresh-keeping for fresh agricultural products according to claim 8, feature exist
In gas bath constant temperature oscillator is shaken in the 20-25 DEG C of speed with 150-300r/min in the step 1.
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