CN106070569B - Core-shell type cyclopropylene antistaling agent and preparation method with sterilization and fresh-keeping double effects - Google Patents
Core-shell type cyclopropylene antistaling agent and preparation method with sterilization and fresh-keeping double effects Download PDFInfo
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- CN106070569B CN106070569B CN201610415317.0A CN201610415317A CN106070569B CN 106070569 B CN106070569 B CN 106070569B CN 201610415317 A CN201610415317 A CN 201610415317A CN 106070569 B CN106070569 B CN 106070569B
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- 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
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- 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
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Abstract
The present invention relates to it is a kind of with sterilization and fresh-keeping double effects core-shell type cyclopropylene antistaling agent and preparation method, core-shell type cyclopropylene antistaling agent percentage, including 45%~50% stratum nucleare, 3%~5% separation layer that can be deliquesced, and 45%~50% shell, and separation layer and shell are successively coated on stratum nucleare from inside to outside；Wherein, stratum nucleare according to parts by weight, including 1~70 part of 1- methyl cyclopropene stable inclusion compound, 10~50 parts of excipient and 1~20 part of sustained release agent；Shell according to parts by weight, including 20~50 parts of chlorite, 5~50 parts of villaumite, 25~45 parts of acidulant and 10~20 parts of effervescent agent.The present invention by mixing core layer material and Shell Materials respectively, then it successively carries out stratum nucleare tabletting, smear separation layer and shell tabletting, the core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects is made, and nucleocapsid efficiently separates, and does not influence each other.
Description
[technical field]
The invention belongs to agricultural product preserving fruit and vegetable utilizing fields, and in particular to a kind of nucleocapsid with sterilization and fresh-keeping double effects
Formula cyclopropylene antistaling agent and preparation method.
[background technique]
Cyclopropene fruit and vegetable fresh-keeping agent, mainly 1- methyl cyclopropene can effectively ethene suppressing pick fruit and vegetable
Dematuration afterwards greatly prolongs the freshness date of picked fruits vegetables.Existing research at present shows through 1- methyl cyclopropene
The bright-coloured of cut-flower can be kept after processing, extend the flower arrangement service life, meanwhile, handling apple, Kiwi berry, persimmon etc. with it can extend
1 times of its post-harvest fresh-keeping phase is more than the time.But 1- methyl cyclopropene is gas at normal temperatures and pressures, in the guarantor to fruit and vegetable
It is also required to use in a gaseous form during fresh, therefore, fruit and vegetable was needed to seal fresh-keeping fruit and vegetable when fresh-keeping, and
It is stored and is transported.This just make it is fresh-keeping after fruit and vegetable be in closed environment, be easy dampness and it is mouldy.Although can reach
Certain fresh-keeping effect, but a large amount of mouldy weaken fresh-keeping effect significantly.
Chlorine dioxide is a kind of internationally recognized safe and nontoxic green sterilization antiseptic.Be highly soluble in water without with water
Reaction, hardly happens hydrolysis.A large amount of experimental study shows that chlorine dioxide is safe and nontoxic disinfectant, nothing both at home and abroad
" three cause " effect (carcinogenic, teratogenesis, mutagenesis), while also chlorination do not occur with organic matter in disinfecting process and generating " three
The organic chloride of cause effect " or other toxic substances.But it since chlorine dioxide has extremely strong oxidability, needs low
It is used under concentration conditions.In terms of any influence, including Physiology and biochemistry will not be generated to human body when concentration is in 100ppm or less
Influence, to skin also without any sensitization.Therefore, chlorine dioxide be widely used in drinking water, health care,
On food and the sterilizing of fruit and vegetable.Chlorine dioxide is all generally immobilized processing for ease of use, it is made
At tablet, if be put into when use in water or wet air can release chlorine dioxide for sterilizing (specially
Sharp CN102246819B, CN104138390A).
When fruit and vegetable fresh-keeping with 1- methyl cyclopropene, need to be sealed it.And fruit and vegetable adopts rear respiration
It is relatively strong, sealing system can be made to become moist through and be conducive to microorganism and grow, cause rotting for fruit and vegetable.This requires fresh-keeping
Sterilizing processing is carried out in the process.Sterilizing first typically is carried out to fruit and vegetable, then carries out fresh-keeping research, entirely
Process is carried out in two steps, this allows for operating process complexity, and is operated to use process more demanding.Existing patent discloses
The cyclopropylene antistaling agent (publication number: CN1505992A) of anti-corrosion and fresh-keeping double effects is prepared, is mainly by antistaling agent and to prevent
Rotten agent is handled respectively and packaging forms A agent and B agent, and use when uses it simultaneously, reaches anti-corrosion and fresh-keeping dual mesh
's.But under 1- methyl cyclopropene normal temperature and pressure it is a kind of very active reducibility gas, it is easy to be oxidized decomposition.And
General sterilization antiseptic has oxidizing component, with 1- methyl cyclopropene simultaneously using being possible to weaken its fresh-keeping effect.
[summary of the invention]
It is an object of the invention to overcome problems of the prior art, provide a kind of with sterilization and fresh-keeping dual effect
The core-shell type cyclopropylene antistaling agent and preparation method of fruit, fungicide and antistaling agent are integrated in one, are independent of each other.
To achieve the goals above, antistaling agent of the present invention adopts the following technical scheme that:
The core-shell type cyclopropylene antistaling agent percentage, including 45%~50% stratum nucleare, 3%~5%
The separation layer that can deliquesce and 45%~50% shell, and separation layer and shell are successively coated on stratum nucleare from inside to outside；
Wherein, stratum nucleare according to parts by weight, including 1~70 part of 1- methyl cyclopropene stable inclusion compound, 10~50 parts
Excipient and 1~20 part of sustained release agent；
Shell according to parts by weight, including 20~50 parts of chlorite, 5~50 parts of villaumite, 25~45 parts of acidification
Agent and 10~20 parts of effervescent agent.
Further, excipient includes glucose, maltose, alpha-cyclodextrin, beta-cyclodextrin, γ cyclodextrin, starch and carboxylic
The mixture of one or more of base cellulose arbitrary proportion.
Further, sustained release agent include one or both of calcium hydroxide, sodium carbonate, sodium bicarbonate and ammonium hydrogen carbonate with
The mixture of upper arbitrary proportion.
Further, separation layer uses cyclodextrin derivative material；Cyclodextrin derivative material includes hydroxy propyl-Beta-ring paste
Essence, methyl-B-cyclodextrin, amino-beta-cyclodextrin, mercapto group-beta-cyclodextrin, malt sugar group-beta-cyclodextrin, hydroxypropyl-α-ring paste
One or both of essence, methyl-alphacyclodextrin, amino-alpha-cyclodextrin, sulfydryl-alpha-cyclodextrin and malt-base-alpha-cyclodextrin
The mixture of any of the above ratio.
Further, chlorite includes sodium chlorite；Villaumite includes anhydrous calcium chloride or sodium chloride；Acidulant includes
Tartaric acid, citric acid or malic acid；Effervescent agent includes sodium bicarbonate, sodium carbonate or ammonium hydrogen carbonate.
Further, the core-shell type cyclopropylene antistaling agent is sheet, and every sheet weight is 0.8~1.2g.
The technical solution of preparation method of the present invention is: the following steps are included:
(1) it takes 1- methyl cyclopropene stable inclusion compound, excipient and sustained release agent to be uniformly mixed and obtains mixture A, will mix
Stratum nucleare tablet is made in object A tabletting；Wherein, 1- methyl cyclopropene stable inclusion compound accounts for the 1%~60% of mixture A weight, figuration
Agent accounts for the 10%~30% of mixture A weight, and sustained release agent accounts for the 1%~20% of mixture A weight；
(2) cyclodextrine derivatives solution is equably coated in stratum nucleare tablet surface and drying and forming-film, in stratum nucleare tablet surface
Form separation layer；
(3) it takes chlorite, villaumite, acidulant and effervescent agent to be uniformly mixed and obtains mixture B, mixture B is wrapped in
The core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects is made in insulation surface and tabletting；Wherein by weight hundred
Score meter, chlorite account for the 20%~50% of mixture B weight, and villaumite accounts for the 5%~45% of mixture B weight, acidulant
The 25%~45% of mixture B weight is accounted for, effervescent agent accounts for the 10%~20% of mixture B weight；
Wherein, mixture A accounts for the 45%~50% of core-shell type cyclopropylene antistaling agent weight, and cyclodextrine derivatives account for core-shell type
The 3%~5% of cyclopropylene antistaling agent weight, mixture B account for the 45%~50% of core-shell type cyclopropylene antistaling agent weight.
Further, in step (1) and step (3) in the environment of 5~35 DEG C of temperature, relative humidity 15~50% into
Row tabletting.
Further, the drying and forming-film of step (2) is dry 30~60min at 30~60 DEG C.
Further, the cyclodextrine derivatives solution of step (2) is that cyclodextrine derivatives are dissolved in solvent to be formed；It is molten
Agent includes the mixture of one or more kinds of arbitrary proportions of methanol, ethyl alcohol, ether, acetone, ethyl acetate, hexamethylene etc.；
The concentration of cyclodextrine derivatives solution is 0.3~0.6g/mL.
Compared with prior art, the invention has the following beneficial technical effects:
The cyclopropylene antistaling agent of core-shell structure prepared by the present invention include the stratum nucleare set gradually from inside to outside, separation layer and
Shell, and separation layer can deliquesce, and have the advantage that
1, the present invention organically combines the fresh-keeping and sterilization and anticorrosion of fruit and vegetable, is respectively formed stratum nucleare and shell, while core
It is separated between shell two parts with separation layer, sterilization is successively carried out with fresh-keeping, and nucleocapsid is made not influence each other.Wherein, Shell Materials are
In use process, antistaling agent of the present invention is placed in a small amount of water or in wet air for sterilization material layer, shell and water or humidity
Air contact first discharges rapidly out chlorine dioxide bactericide, realizes the sterilization and anticorrosion of fruit and vegetable, after to be sterilized, separation layer
It is easily dissolved by water or humid air, ineffective, stratum nucleare contact water or humid air start slow release 1- methyl cyclopropyl later
Alkene antistaling agent gas carries out fruit and vegetable fresh-keeping.The chlorine dioxide (oxidant) that shell generates when fresh-keeping consumes substantially
Complete, the 1- methyl cyclopropene (reducing agent) that will not be generated to stratum nucleare has an impact；
2, stratum nucleare and shell are efficiently separated using cyclodextrin substance in the preparation process of antistaling agent, is sealing it
It will not contact with each other and react during storage and transport, ensure that the stability of this antistaling agent with double action；
3, the environment-friendly and green Chlorine Dioxide In Disinfectant generally acknowledged using the World Health Organization has broad-spectrum sterilization, and dosage is low,
The advantages that work fast, bactericidal effect are good, length of holding time, without secondary pollution；
4, using 1- methyl cyclopropene antistaling agent, have many advantages, such as that dosage is low, of good preservation effect, green non-pollution.
First 1- methyl cyclopropene stable inclusion compound and certain excipient, sustained release agent are mixed in preparation method of the present invention equal
Even, then tabletting forms the core layer material with preservation, wraps up one layer of cyclodextrine derivatives on stratum nucleare surface.Then exist
The outer layer of antistaling agent piece after package encloses one layer of Shell Materials that can generate sterilization by way of tabletting again, is finally made
Core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects, preparation method is simple, by the sterilization and anticorrosion of fruits and vegetables and guarantor
It is fresh to be integrated in one, make same material that there is fresh-keeping and sterilization double action, and fresh-keeping part and the barrier well of sterilization part
It will not influence each other.
[Detailed description of the invention]
Fig. 1 is the structural schematic diagram of nucleocapsid antistaling agent of the present invention；
Fig. 2 is the sectional view of nucleocapsid antistaling agent of the present invention.
Wherein, 1- shell；2- separation layer；3- stratum nucleare.
[specific implementation method]
It elaborates with reference to the accompanying drawing to the present invention.
The present invention has the core-shell type cyclopropylene antistaling agent of sterilization and fresh-keeping double action, is divided into stratum nucleare antistaling agent part
Part is sterilized with shell, and the material that can generate preservation must can generate bactericidal effect as nucleome material
Material needs to be obstructed using certain substance as case material, between nucleome and shell, to prevent between the two directly
It contacts and reacts, guarantee to organically combine both fresh-keeping and sterilization and anticorrosions, but do not influence each other.
Referring to Fig. 1 and Fig. 2, core-shell type cyclopropylene antistaling agent of the present invention is sheet, and including successively coating from outside to inside
Shell 1, separation layer 2 and stratum nucleare 3, wherein the weight of stratum nucleare 3 and shell 1 accounts for 45%~50% or so of full wafer weight respectively,
And separation layer 2 accounts for the 3%~5% of full wafer weight.
Core layer material is mainly the material that can generate 1- methyl cyclopropene fruit and vegetable fresh-keeping agent, according to parts by weight, including 1~
70 parts of cyclopropylene inclusion complex, 10~50 parts of excipient and 1~20 part of sustained release agent.Cyclopropylene inclusion complex is 1- methyl cyclopropyl
Alkene stable inclusion compound (i.e. the stable inclusion compound of the preparation of patent 200610042683.2)；Excipient is glucose, maltose, α-ring
One or more cooperations of dextrin, beta-cyclodextrin, γ cyclodextrin, starch, carboxycellulose etc.；Sustained release agent is calcium hydroxide, carbon
One of sour sodium, sodium bicarbonate, ammonium hydrogen carbonate or a variety of cooperations.
Isolated material between nucleocapsid is mainly deliquescent cyclodextrin derivative material, including hydroxypropyl-β-cyclodextrin,
Methyl-B-cyclodextrin, amino-beta-cyclodextrin, mercapto group-beta-cyclodextrin, malt sugar group-beta-cyclodextrin, Hydroxyproply-α-cyclodextrin,
The one or more of methyl-alphacyclodextrin, amino-alpha-cyclodextrin, sulfydryl-alpha-cyclodextrin, malt-base-alpha-cyclodextrin etc. mix
It closes.
Shell Materials are mainly the material for generating chlorine dioxide bactericide, according to parts by weight, including 20~50 parts of Asia
Chlorate, 5~50 parts of villaumite, 25~45 parts of acidulant, 10~20 parts of effervescent agent etc..Wherein chlorite is mainly Asia
Sodium chlorate, villaumite are mainly anhydrous calcium chloride or sodium chloride, and acidulant is mainly that tartaric acid, citric acid and malic acid etc. are organic
Acid, effervescent agent are mainly sodium bicarbonate, sodium carbonate or ammonium hydrogen carbonate etc..
Preparation method of the present invention includes the following steps:
Stratum nucleare tabletting: firstly, 1- methyl cyclopropene stable inclusion compound and certain excipient, sustained release agent are uniformly mixed,
In the environment of 5~35 DEG C of temperature, relative humidity 15~50%, the mixture of core layer material is pressed on tablet press machine using punch die
The tablet of weight about 0.5g is made, forms the stratum nucleare tablet with preservation.
The coating of intermediate isolating layer: cyclodextrine derivatives are dissolved in the height that 0.3~0.6g/mL is made in volatile solvent
Then the solution of the cyclodextrine derivatives dissolved is equably coated in the stratum nucleare tablet surface suppressed simultaneously by concentration viscous solution
Dry 30~60min at 30~60 DEG C forms one layer of very thin film in stratum nucleare tablet surface, and protection core layer material will not be with shell
Layer material contact and reaction；Used easy volatile solvent is methanol, ethyl alcohol, ether, acetone, ethyl acetate, hexamethylene etc.
One or more of mixing.
Shell tabletting: after intermediate isolating layer material is coated and dried, (about by the Shell Materials mixed in proportion
0.5g) in the environment of 5~35 DEG C of temperature, relative humidity 15~50%, package stratum nucleare tablet is pressed into finally on tablet press machine
The tablet of 0.8~1.2g of weight.
The present invention by by patent (200610042683.2) 1- methyl cyclopropene stable inclusion compound and certain tax
Shape agent, sustained release agent are uniformly mixed, and are then pressed into small pieces, form the core layer material with preservation, wrap up one on stratum nucleare surface
Layer cyclodextrine derivatives.Then the outer layer of the antistaling agent piece after package, which is enclosed one layer by way of tabletting again and can be generated, kills
The chlorine dioxide material of bacterium.It is finally made the core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects.
The present invention is described in further details below by specific embodiment.
Embodiment 1
(1) the 1- methyl cyclopropene stable inclusion compound of 1 dry parts by weight, the excipient and 5 parts by weight of 10 parts by weight are taken
Sustained release agent powder, poured out after mixing 30min in three-dimensional motion mixer, obtain mixture A, at 5 DEG C of temperature, relative humidity
In the environment of 15%, by mixture A, stratum nucleare tablet is made in tabletting in tablet press machine；Wherein, excipient uses glucose；Sustained release agent
Using sodium bicarbonate；
(2) hydroxypropyl-β-cyclodextrin is dissolved in the high concentration viscous solution that 0.5g/mL is made in dehydrated alcohol, with hair
Hydroxypropyl-β-cyclodextrin solution lightly, is equably coated in stratum nucleare tablet surface by brush, and dries 60min in 50 DEG C of baking ovens
Film forming forms separation layer in stratum nucleare tablet surface, obtains the tablet with separation layer；
(3) take the sodium chlorite of 20 dry parts by weight, the anhydrous calcium chloride of 20 parts by weight, 30 parts by weight citric acid and
The sodium bicarbonate of 10 parts by weight is poured out after mixing 30min in three-dimensional motion mixer, obtains mixture B, at 5 DEG C of temperature, phase
In the environment of humidity 15%, the tablet with separation layer that step (2) prepares is placed in mixture B, and in tablet press machine
The core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects is made in middle tabletting.
Obtained core-shell type cyclopropylene antistaling agent weight is 1.0g/ piece, and mixture A accounts for core-shell type cyclopropylene antistaling agent weight
The 47% of amount, cyclodextrine derivatives account for the 3% of core-shell type cyclopropylene antistaling agent weight, and it is fresh-keeping that mixture B accounts for core-shell type cyclopropylene
The 50% of agent weight.
Embodiment 2
(1) the 1- methyl cyclopropene stable inclusion compound of 5 dry parts by weight, the excipient and 10 parts by weight of 20 parts by weight are taken
Sustained release agent powder, in three-dimensional motion mixer mix 30min after pour out, obtain mixture A, it is relatively wet at 10 DEG C of temperature
In the environment of degree 20%, by mixture A, stratum nucleare tablet is made in tabletting in tablet press machine；Wherein, excipient uses starch；Sustained release agent
Using sodium carbonate；
(2) methyl-B-cyclodextrin is dissolved in the high concentration viscous solution that 0.4g/mL is made in dehydrated alcohol, with hairbrush
Methyl-B-cyclodextrin solution lightly, is equably coated in stratum nucleare tablet surface, and dries 50min film forming in 40 DEG C of baking ovens,
Separation layer is formed in stratum nucleare tablet surface, obtains the tablet with separation layer；
(3) take the sodium chlorite of 30 dry parts by weight, the sodium chloride of 15 parts by weight, 40 parts by weight tartaric acid and 11 weights
The sodium carbonate of amount part is poured out after mixing 30min in three-dimensional motion mixer, obtains mixture B, at 10 DEG C of temperature, relative humidity
In the environment of 20%, the tablet with separation layer that step (2) prepares is placed in mixture B, and the tabletting in tablet press machine,
The core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects is made.
Obtained core-shell type cyclopropylene antistaling agent weight is 0.9g/ piece, and mixture A accounts for core-shell type cyclopropylene antistaling agent weight
The 45% of amount, cyclodextrine derivatives account for the 5% of core-shell type cyclopropylene antistaling agent weight, and it is fresh-keeping that mixture B accounts for core-shell type cyclopropylene
The 50% of agent weight.
The antistaling agent of core-shell structure of the present invention is in use, it is only necessary to be directly added into a small amount of water, to being placed with water
After handling 8-12h in the confined space of fruit vegetable, the container for filling antistaling agent is taken out, using simple.Table 1 is this implementation
Antistaling agent made from example is compared with the effect of individual 1- methyl cyclopropene antistaling agent and chlorine dioxide tablet processing Kiwi berry.Knot
Fruit shows that the present invention obtained has the core-shell type antistaling agent and existing antistaling agent and fungicide of sterilization and fresh-keeping double effects
It compares, has effectively contained the mouldy of persimmon, the fresh-keeping of persimmon has been better achieved.
Table 1 has the core-shell type cyclopropylene antistaling agent of sterilization and fresh-keeping double effects to persimmon treatment effect (room temperature 32
It)
| Inorganic agent | Fruit color | The mouldy rate (%) of corruption | The hardness of fruit (Kg/cm) |
| The present invention | Yellow | 0 | 12.7 (hard) |
| 1- methyl cyclopropene | Yellow | 13.8% | 10.2 (hard) |
| Chlorine dioxide | It is orange red | 0 | 5.6 (partially soft) |
| Control | Peony | 28.7% | 2.1 (very soft) |
Embodiment 3
(1) the 1- methyl cyclopropene stable inclusion compound of 10 dry parts by weight, the excipient and 1 parts by weight of 30 parts by weight are taken
Sustained release agent powder, in three-dimensional motion mixer mix 30min after pour out, obtain mixture A, it is relatively wet at 15 DEG C of temperature
In the environment of degree 50%, by mixture A, stratum nucleare tablet is made in tabletting in tablet press machine；Wherein, excipient uses maltose；Sustained release
Agent uses calcium hydroxide；
(2) amino-beta-cyclodextrin is made to the high concentration viscous solution of 0.3g/mL in methyl alcohol, with hairbrush by ammonia
Group-beta-cyclodextrin solution lightly, is equably coated in stratum nucleare tablet surface, and 40min film forming is dried in 60 DEG C of baking ovens, in core
Layer tablet surface forms separation layer, obtains the tablet with separation layer；
(3) take the sodium chlorite of 40 dry parts by weight, the sodium chloride of 5 parts by weight, 25 parts by weight malic acid and 12 weights
The ammonium hydrogen carbonate of amount part is poured out after mixing 30min in three-dimensional motion mixer, obtains mixture B, relatively wet at 15 DEG C of temperature
In the environment of degree 50%, the tablet with separation layer that step (2) prepares is placed in mixture B, and is pressed in tablet press machine
The core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects is made in piece.
Obtained core-shell type cyclopropylene antistaling agent weight is 1.1g/ piece, and mixture A accounts for core-shell type cyclopropylene antistaling agent weight
The 50% of amount, cyclodextrine derivatives account for the 5% of core-shell type cyclopropylene antistaling agent weight, and it is fresh-keeping that mixture B accounts for core-shell type cyclopropylene
The 45% of agent weight.
Embodiment 4
(1) the 1- methyl cyclopropene stable inclusion compound of 20 dry parts by weight, the excipient and 15 weight of 40 parts by weight are taken
The sustained release agent powder of part is poured out after mixing 30min in three-dimensional motion mixer, obtains mixture A, at 20 DEG C of temperature, relatively
In the environment of humidity 45%, by mixture A, stratum nucleare tablet is made in tabletting in tablet press machine；Wherein, excipient uses alpha-cyclodextrin
The mixture mixed with beta-cyclodextrin with arbitrary proportion；Sustained release agent uses ammonium hydrogen carbonate；
(2) mercapto group-beta-cyclodextrin is dissolved in the high concentration viscous solution that 0.35g/mL is made in ether, with hairbrush by mercapto
Group-beta-cyclodextrin solution lightly, is equably coated in stratum nucleare tablet surface, and 55min film forming is dried in 30 DEG C of baking ovens, in core
Layer tablet surface forms separation layer, obtains the tablet with separation layer；
(3) take the sodium chlorite of 50 dry parts by weight, the sodium chloride of 10 parts by weight, 35 parts by weight citric acid and 15 weights
The ammonium hydrogen carbonate of amount part is poured out after mixing 30min in three-dimensional motion mixer, obtains mixture B, relatively wet at 20 DEG C of temperature
In the environment of degree 45%, the tablet with separation layer that step (2) prepares is placed in mixture B, and is pressed in tablet press machine
The core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects is made in piece.
Obtained core-shell type cyclopropylene antistaling agent weight is 0.8g/ piece, and mixture A accounts for core-shell type cyclopropylene antistaling agent weight
The 48% of amount, cyclodextrine derivatives account for the 4% of core-shell type cyclopropylene antistaling agent weight, and it is fresh-keeping that mixture B accounts for core-shell type cyclopropylene
The 48% of agent weight.
Embodiment 5
(1) the 1- methyl cyclopropene stable inclusion compound of 30 dry parts by weight, the excipient and 20 weight of 50 parts by weight are taken
The sustained release agent powder of part is poured out after mixing 30min in three-dimensional motion mixer, obtains mixture A, at 25 DEG C of temperature, relatively
In the environment of humidity 35%, by mixture A, stratum nucleare tablet is made in tabletting in tablet press machine；Wherein, excipient uses carboxylated fiber
Element；The mixture that sustained release agent uses calcium hydroxide and sodium carbonate to mix with arbitrary proportion；
(2) cyclodextrine derivatives are dissolved in the high concentration viscous solution that 0.45g/mL is made in ethyl acetate, with hairbrush
Cyclodextrine derivatives solution lightly, is equably coated in stratum nucleare tablet surface, and dries 45min film forming in 35 DEG C of baking ovens,
Separation layer is formed in stratum nucleare tablet surface, obtains the tablet with separation layer；Cyclodextrine derivatives use malt sugar group-beta-cyclodextrin
The mixture mixed with Hydroxyproply-α-cyclodextrin with arbitrary proportion；
(3) take the sodium chlorite of 25 dry parts by weight, the sodium chloride of 30 parts by weight, 45 parts by weight tartaric acid and 20 weights
The sodium bicarbonate of amount part is poured out after mixing 30min in three-dimensional motion mixer, obtains mixture B, relatively wet at 25 DEG C of temperature
In the environment of degree 35%, the tablet with separation layer that step (2) prepares is placed in mixture B, and is pressed in tablet press machine
The core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects is made in piece.
Obtained core-shell type cyclopropylene antistaling agent weight is 1.2g/ piece, and mixture A accounts for core-shell type cyclopropylene antistaling agent weight
The 46% of amount, cyclodextrine derivatives account for the 4% of core-shell type cyclopropylene antistaling agent weight, and it is fresh-keeping that mixture B accounts for core-shell type cyclopropylene
The 50% of agent weight.
Embodiment 6
(1) the 1- methyl cyclopropene stable inclusion compound of 40 dry parts by weight, the excipient and 18 weight of 45 parts by weight are taken
The sustained release agent powder of part is poured out after mixing 30min in three-dimensional motion mixer, obtains mixture A, at 30 DEG C of temperature, relatively
In the environment of humidity 40%, by mixture A, stratum nucleare tablet is made in tabletting in tablet press machine；Wherein, excipient using glucose and
The mixture that maltose is mixed with arbitrary proportion；The mixing that sustained release agent uses sodium bicarbonate and ammonium hydrogen carbonate to mix with arbitrary proportion
Object；
(2) the high concentration viscous solution of 0.55g/mL is made in cyclodextrine derivatives dissolution in a solvent, with hairbrush by ring
Dextrin derivative solution lightly, is equably coated in stratum nucleare tablet surface, and 35min film forming is dried in 45 DEG C of baking ovens, in core
Layer tablet surface forms separation layer, obtains the tablet with separation layer；Cyclodextrine derivatives use amino-alpha-cyclodextrin；Ethyl alcohol and
The mixture that ethyl acetate is mixed with arbitrary proportion；
(3) take the sodium chlorite of 35 dry parts by weight, the anhydrous calcium chloride of 40 parts by weight, 32 parts by weight malic acid and
The sodium carbonate of 18 parts by weight is poured out after mixing 30min in three-dimensional motion mixer, obtains mixture B, at 30 DEG C of temperature, relatively
In the environment of humidity 40%, the tablet with separation layer that step (2) prepares is placed in mixture B, and in tablet press machine
The core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects is made in tabletting.
Obtained core-shell type cyclopropylene antistaling agent weight is 0.8g/ piece, and mixture A accounts for core-shell type cyclopropylene antistaling agent weight
The 49% of amount, cyclodextrine derivatives account for the 3% of core-shell type cyclopropylene antistaling agent weight, and it is fresh-keeping that mixture B accounts for core-shell type cyclopropylene
The 48% of agent weight.
Embodiment 7
(1) the 1- methyl cyclopropene stable inclusion compound of 50 dry parts by weight, the excipient and 14 weight of 35 parts by weight are taken
The sustained release agent powder of part is poured out after mixing 30min in three-dimensional motion mixer, obtains mixture A, at 35 DEG C of temperature, relatively
In the environment of humidity 30%, by mixture A, stratum nucleare tablet is made in tabletting in tablet press machine；Wherein, excipient uses starch and carboxylic
The mixture that base cellulose is mixed with arbitrary proportion；Sustained release agent uses sodium carbonate, sodium bicarbonate and ammonium hydrogen carbonate with arbitrary proportion
Mixed mixture；
(2) cyclodextrine derivatives dissolution is made to the high concentration viscous solution of 0.6g/mL in a solvent, is pasted ring with hairbrush
Smart derivative solution lightly, is equably coated in stratum nucleare tablet surface, and 30min film forming is dried in 55 DEG C of baking ovens, in stratum nucleare
Tablet surface forms separation layer, obtains the tablet with separation layer；Cyclodextrine derivatives use amino-alpha-cyclodextrin；Solvent uses
The mixture that ethyl alcohol and ethyl acetate are mixed with arbitrary proportion；
(3) take the sodium chlorite of 45 dry parts by weight, the anhydrous calcium chloride of 50 parts by weight, 38 parts by weight citric acid and
The ammonium hydrogen carbonate of 16 parts by weight is poured out after mixing 30min in three-dimensional motion mixer, obtains mixture B, at 35 DEG C of temperature, phase
In the environment of humidity 30%, the tablet with separation layer that step (2) prepares is placed in mixture B, and in tablet press machine
The core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects is made in middle tabletting.
Obtained core-shell type cyclopropylene antistaling agent weight is 0.9g/ piece, and mixture A accounts for core-shell type cyclopropylene antistaling agent weight
The 48% of amount, cyclodextrine derivatives account for the 3% of core-shell type cyclopropylene antistaling agent weight, and it is fresh-keeping that mixture B accounts for core-shell type cyclopropylene
The 49% of agent weight.
Embodiment 8
(1) the 1- methyl cyclopropene stable inclusion compound of 60 dry parts by weight, the excipient and 8 parts by weight of 25 parts by weight are taken
Sustained release agent powder, in three-dimensional motion mixer mix 30min after pour out, obtain mixture A, it is relatively wet at 20 DEG C of temperature
In the environment of degree 25%, by mixture A, stratum nucleare tablet is made in tabletting in tablet press machine；Wherein, excipient uses glucose, malt
The mixture that sugar and carboxylated fiber are mixed with arbitrary proportion；Sustained release agent uses calcium hydroxide, sodium carbonate, sodium bicarbonate and bicarbonate
The mixture that ammonium is mixed with arbitrary proportion；
(2) cyclodextrine derivatives dissolution is made to the high concentration viscous solution of 0.4g/mL in a solvent, is pasted ring with hairbrush
Smart derivative solution lightly, is equably coated in stratum nucleare tablet surface, and 40min film forming is dried in 40 DEG C of baking ovens, in stratum nucleare
Tablet surface forms separation layer, obtains the tablet with separation layer；Cyclodextrine derivatives use methyl-B-cyclodextrin, amino-beta-ring
The mixture that dextrin, Hydroxyproply-α-cyclodextrin and methyl-alphacyclodextrin are mixed with arbitrary proportion；Solvent using ethyl acetate and
The mixture that hexamethylene is mixed with arbitrary proportion；
(3) take the sodium chlorite of 35 dry parts by weight, the anhydrous calcium chloride of 25 parts by weight, 44 parts by weight tartaric acid and
The sodium bicarbonate of 15 parts by weight is poured out after mixing 30min in three-dimensional motion mixer, obtains mixture B, at 20 DEG C of temperature, phase
In the environment of humidity 25%, the tablet with separation layer that step (2) prepares is placed in mixture B, and in tablet press machine
The core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects is made in middle tabletting.
Obtained core-shell type cyclopropylene antistaling agent weight is 1.0g/ piece, and mixture A accounts for core-shell type cyclopropylene antistaling agent weight
The 50% of amount, cyclodextrine derivatives account for the 4% of core-shell type cyclopropylene antistaling agent weight, and it is fresh-keeping that mixture B accounts for core-shell type cyclopropylene
The 46% of agent weight.
Embodiment 9
(1) the 1- methyl cyclopropene stable inclusion compound of 70 dry parts by weight, the excipient and 3 parts by weight of 15 parts by weight are taken
Sustained release agent powder, in three-dimensional motion mixer mix 30min after pour out, obtain mixture A, it is relatively wet at 25 DEG C of temperature
In the environment of degree 30%, by mixture A, stratum nucleare tablet is made in tabletting in tablet press machine；Wherein, excipient uses glucose, malt
The mixture that sugar, alpha-cyclodextrin, beta-cyclodextrin and γ cyclodextrin are mixed with arbitrary proportion；Sustained release agent uses sodium bicarbonate；
(2) malt-base-alpha-cyclodextrin dissolution is made to the high concentration viscous solution of 0.3g/mL in a solvent, with hairbrush
Malt-base-alpha-cyclodextrin solution lightly, is equably coated in stratum nucleare tablet surface, and dries 50min in 50 DEG C of baking ovens
Film forming forms separation layer in stratum nucleare tablet surface, obtains the tablet with separation layer；Solvent uses methanol, ethyl alcohol and ether to appoint
The mixture of meaning ratio mixing；
(3) take the sodium chlorite of 30 dry parts by weight, the anhydrous calcium chloride of 35 parts by weight, 26 parts by weight malic acid and
The sodium carbonate of 19 parts by weight is poured out after mixing 30min in three-dimensional motion mixer, obtains mixture B, relatively wet in 30 DEG C of temperature
In the environment of degree 25%, the tablet with separation layer that step (2) prepares is placed in mixture B, and is pressed in tablet press machine
The core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects is made in piece.
Obtained core-shell type cyclopropylene antistaling agent weight is 1.2g/ piece, and mixture A accounts for core-shell type cyclopropylene antistaling agent weight
The 48% of amount, cyclodextrine derivatives account for the 5% of core-shell type cyclopropylene antistaling agent weight, and it is fresh-keeping that mixture B accounts for core-shell type cyclopropylene
The 47% of agent weight.
The method of antistaling agent of the present invention is the following steps are included: (1) drying materials；(2) core layer material and Shell Materials difference
Mixing, (3) core layer material tabletting；(4) nucleocapsid isolated material is smeared；(5) Shell Materials tabletting.It is prepared by the present invention that there is sterilization
Be placed in water or wet air with the core-shell type cyclopropylene antistaling agent of fresh-keeping double action to release (within 1~2min) quickly
Chlorine dioxide is released, bactericidal effect is played.1- methylcyclopropene gas fruit and vegetable fresh-keeping agent can be released again after 2-3h, is risen
To the preservation of fruits and vegetables.It is easy to use its advantage is that carry out the sterilization of fruits and vegetables and a fresh-keeping step, and will not to human body and
Environment causes damages.
Claims (9)
1. the core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects, it is characterised in that: the core-shell type cyclopropyl
Alkene antistaling agent percentage, including 45%~50% stratum nucleare, 3%~5% separation layer that can be deliquesced and 45%
~50% shell, and separation layer and shell are successively coated on stratum nucleare from inside to outside；
Wherein, stratum nucleare according to parts by weight, including 1~70 part of 1- methyl cyclopropene stable inclusion compound, 10~50 parts of figuration
Agent and 1~20 part of sustained release agent；
Shell according to parts by weight, including 20~50 parts of chlorite, 5~50 parts of villaumite, 25~45 parts of acidulant, with
And 10~20 parts of effervescent agent；
Separation layer uses cyclodextrin derivative material；Cyclodextrin derivative material includes hydroxypropyl-β-cyclodextrin, methyl-β-ring
Dextrin, amino-beta-cyclodextrin, mercapto group-beta-cyclodextrin, malt sugar group-beta-cyclodextrin, Hydroxyproply-α-cyclodextrin, methyl-α-ring
One or more of dextrin, amino-alpha-cyclodextrin, sulfydryl-alpha-cyclodextrin and malt-base-alpha-cyclodextrin arbitrary proportion
Mixture.
2. the core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects according to claim 1, feature exist
In: excipient includes one in glucose, maltose, alpha-cyclodextrin, beta-cyclodextrin, γ cyclodextrin, starch and carboxycellulose
The mixture of kind or two or more arbitrary proportions.
3. the core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects according to claim 1, feature exist
In: sustained release agent includes the mixed of one or more of calcium hydroxide, sodium carbonate, sodium bicarbonate and ammonium hydrogen carbonate arbitrary proportion
Close object.
4. the core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects according to claim 1, feature exist
In: chlorite includes sodium chlorite；Villaumite includes anhydrous calcium chloride or sodium chloride；Acidulant includes tartaric acid, citric acid
Or malic acid；Effervescent agent includes sodium bicarbonate, sodium carbonate or ammonium hydrogen carbonate.
5. the core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects according to claim 1, feature exist
In: the core-shell type cyclopropylene antistaling agent is sheet, and every sheet weight is 0.8~1.2g.
6. have sterilization and fresh-keeping double effects core-shell type cyclopropylene antistaling agent preparation method, it is characterised in that: including with
Lower step:
(1) it takes 1- methyl cyclopropene stable inclusion compound, excipient and sustained release agent to be uniformly mixed and obtains mixture A, mixture A is pressed
Stratum nucleare tablet is made in piece；Wherein, 1- methyl cyclopropene stable inclusion compound accounts for the 1%~60% of mixture A weight, and excipient accounts for mixed
The 10%~30% of object A weight is closed, sustained release agent accounts for the 1%~20% of mixture A weight；
(2) cyclodextrine derivatives solution is equably coated in stratum nucleare tablet surface and drying and forming-film, is formed in stratum nucleare tablet surface
Separation layer；
(3) it takes chlorite, villaumite, acidulant and effervescent agent to be uniformly mixed and obtains mixture B, mixture B is wrapped in isolation
The core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects is made in layer surface and tabletting；Wherein weight percent
Meter, chlorite account for the 20%~50% of mixture B weight, and villaumite accounts for the 5%~45% of mixture B weight, and acidulant accounts for mixed
The 25%~45% of object B weight is closed, effervescent agent accounts for the 10%~20% of mixture B weight；
Wherein, mixture A accounts for the 45%~50% of core-shell type cyclopropylene antistaling agent weight, and cyclodextrine derivatives account for core-shell type cyclopropyl
The 3%~5% of alkene antistaling agent weight, mixture B account for the 45%~50% of core-shell type cyclopropylene antistaling agent weight.
7. the preparation side of the core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects according to claim 6
Method, it is characterised in that: carried out in the environment of 5~35 DEG C of temperature, relative humidity 15~50% in step (1) and step (3)
Tabletting.
8. the preparation side of the core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects according to claim 6
Method, it is characterised in that: the drying and forming-film of step (2) is dry 30~60min at 30~60 DEG C.
9. the preparation side of the core-shell type cyclopropylene antistaling agent with sterilization and fresh-keeping double effects according to claim 6
Method, it is characterised in that: the cyclodextrine derivatives solution of step (2) is that cyclodextrine derivatives are dissolved in solvent to be formed；Solvent
The mixture of one or more kinds of arbitrary proportions including methanol, ethyl alcohol, ether, acetone, ethyl acetate, hexamethylene etc.；Ring
The concentration of dextrin derivative solution is 0.3~0.6g/mL.
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| CN113367153A (en) * | 2021-06-04 | 2021-09-10 | 湖南天为环保科技有限公司 | Deodorant based on chlorine dioxide |
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| CN100364394C (en) * | 2005-08-05 | 2008-01-30 | 高荣涛 | Microcapsuled fruit, vegetable and flower antistaling agent and preparation thereof |
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