CN110214919A - A kind of high embedding essence microcapsule and preparation method thereof - Google Patents
A kind of high embedding essence microcapsule and preparation method thereof Download PDFInfo
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- CN110214919A CN110214919A CN201910605711.4A CN201910605711A CN110214919A CN 110214919 A CN110214919 A CN 110214919A CN 201910605711 A CN201910605711 A CN 201910605711A CN 110214919 A CN110214919 A CN 110214919A
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/70—Fixation, conservation, or encapsulation of flavouring agents
- A23L27/72—Encapsulation
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/30—Encapsulation of particles, e.g. foodstuff additives
Abstract
The invention discloses a kind of high embedding essence microcapsules and preparation method thereof.The preparation method mixes maltodextrin with porous-starch；Distilled water is added to be stirred and is made into mixed liquor, crosslinking agent is added, adjust pH of mixed be 9~11,30~60 DEG C be stirred to react the time be 4~for 24 hours, adjust pH of mixed to 7~8, washing, it is dry, crush, be sieved after obtain essence wall material；Essence is added in wall material solution, homogeneous forms uniform emulsion, is spray-dried and essence microcapsule is made.Product Green environmental protection of the invention, at low cost, the essence embedding rate after microcapsules absorption is above 85%, and the peroxide value after 60 DEG C of oxidation 12d is lower than 0.15g/100g.This method embedding essence can improve the embedding rate of essence, delay the oxidation of essence, be conducive to the storage transport and its application of essence.
Description
Technical field
The present invention relates to the technical fields of flavors and fragrances processing, more particularly to a kind of high embedding essence microcapsule and its system
Preparation Method.
Background technique
The aroma substance that edible essence refers to the fragrance with natural melon and fruit etc. and can be eaten, edible essence can be with
Raw-food material fragrance is assigned, the deficiency of fragrance in food is made up, the flavor of food is made to be improved and be optimized, therefore answered extensively
For modern food industry.The feeling of olfactory organ is pressed, essence can be divided into fragrant head, body note and basic note.Soluble perfume be by
Natural perfume material, synthetic perfume are dissolved made of reconciling with ethanol water (or other water-soluble solvents such as propylene glycol), main
It is used in soft drink, drinks etc..
For common essence mostly by material compositions such as alcohol, aldehyde, ketone, acid and esters, these substances have lower boiling point, and are permitted
More substances all contain unsaturated bond, thus they to it is damp and hot it is sensitive, be easy to volatilize, oxidizable, easy with other component reactions etc.,
Loss in food processing and storage process frequent occurrence, can be very good to protect these substances using state-of-the-art technology, improve
Its stability and processability.Microcapsules technology is the method for common embedding essence, and microencapsulation processing is conducive to improve essence
Stability.There are many substance that can be used as microcapsule wall material, and common wall material can be divided into carbohydrate by its chemical property
Class, such as starch, corn syrup solids, maltodextrin, chitosan, small molecule carbohydrate, sodium alginate and various natural plant gum class (we
Primary glue, carragheen, carrageenan, xanthan gum, pectin etc.)；It is protein-based, such as soybean protein, gelatin, zein, lactalbumin
Deng；Wax and lipid material, such as beeswax, paraffin, grease, liposome.In recent years, the patent of various microcapsule wall material embedding essence
And article has been reported that more, is concentrated mainly on and improves its slow-release and embedding rate etc..
Chinese invention patent 2011104404693 discloses one kind with Arabic gum and beta-cyclodextrin or Arabic gum malt
The wall material solution of dextrin or Arabic gum porous-starch, blackberry anthocyanin extract are core material, are sprayed after anticaking agent is added
The microcapsules of dry preparation；Chinese invention patent application 2014107000553 discloses one kind by Rana oil polypeptide core material 10-
20%, maltodextrin 30-50%, sodium carboxymethylcellulose 10-20%, beta-cyclodextrin 5-20%, porous-starch 5-10% preparation
Microcapsules.But the core material embedding rate of such technology needs to be further increased, and such technology is mainly using embedding pair
Core material protection, although being conducive to that core material is avoided directly to contact the external world, to certain protection is contacted with oxygen, there is no consider
The performance characteristic of wall material itself, as wall material it is heat-insulated, be protected from light, oxygen-impermeable comprehensive performance, for simultaneously it is all quick to light, heat, oxygen
The core material protection of sense is limited.
Summary of the invention
All there is preferable protection, and high packet to light, heat, oxygen technical problem to be solved by the invention is to provide a kind of
Essence microcapsule buried and preparation method thereof, essence microcapsule Product Green environmental protection prepared by the present invention, at low cost, the essence
The essence embedding rate of microcapsules is above 85%, and the peroxide value after 60 DEG C of oxidation 12d is lower than 0.15g/100g.
The present invention can use a variety of different starch, such as cornstarch, wax using renewable resource starch as raw material
Matter cornstarch, potato starch, pea starch, rice starch etc..Malt paste is prepared after different enzymatic hydrolysis with starch
Essence and porous-starch.Due to all having hydroxyl on maltodextrin and porous-starch, the substance containing binary or polynary functional group (is handed over
Connection agent) it can be reacted with maltodextrin and porous-starch.Cross-linking reaction makes porous-starch molecule, maltodextrin molecule in the molecule
Or it is intermolecular react, form a kind of tridimensional network, on the one hand this tridimensional network can enhance the absorption of starch
Property, porous-starch and maltodextrin on the other hand can be made to link together, so that the mixture embeddability properties that reaction obtains improve.
Emulsifier is added in core material and wall material, emulsifier is conducive to the difference in core material and wall material due to its good amphipathic property
Constituent substance forms uniform emulsion, is conducive to protect essence in spray drying, effectively essence can be avoided in high temperature
Lower volatilization oxidation, improves the embedding rate of microcapsules.
The object of the invention is achieved through the following technical solutions:
A kind of preparation method of high embedding essence microcapsule, comprising the following steps:
(1) preparation of maltodextrin: starch adds water to be made into the starch milk of 30%~45% mass fraction, and being adjusted to pH value of solution is
4.5~6.5, alpha-amylase is added, after 70~90 DEG C of 20~60min of holding, reduces temperature to 60~75 DEG C, continues conversion extremely
For DE value to 11~17, enzyme deactivation stops conversion；It is spray-dried that white fine powder is made, obtain maltodextrin；
(2) preparation of porous-starch: being made into starch milk with sodium-acetate buffer for starch, in 45~60 DEG C of stirred in water bath
Mix preheating after, be added mixed enzyme, reaction 6~for 24 hours after, be adjusted to pH be 7~8；Washing, dry, sieving obtains porous-starch；Institute
The mixed enzyme stated is mixed by 1:1~3:1 mass ratio with amyloglucosidase by alpha-amylase and is formed；
(3) preparation of essence wall material: maltodextrin is mixed with porous-starch；Addition distilled water, which is stirred, is made into mixing
Crosslinking agent is added in liquid, adjust pH of mixed be 9~11,30~60 DEG C be stirred to react the time be 4~for 24 hours, adjusting pH of mixed to
7~8, essence wall material is obtained after washing, dry, crushing, sieving；The crosslinking agent is sodium trimetaphosphate, phosphorus oxychloride and epoxy
One of chloropropane is a variety of；
(4) it the preparation of essence microcapsule: takes essence wall material that the solution that distilled water is made into 20~40% is added, adds 0.5
~2% emulsifier, which heats up to stir in water bath with thermostatic control, dissolves it sufficiently, is cooled to room temperature, obtains wall material solution；It will be water-soluble
Essence is added in wall material solution, and homogeneous forms uniform emulsion, spray drying, and the powdery, water-soluble for obtaining solid-state mobility is fragrant
Precise and tiny capsule；The emulsifier is a kind of in neopelex, neopelex and alkylbenzene naphthenic acid sodium
Or it is a variety of.
To further realize the object of the invention, it is preferable that in step (1), the additional amount of the alpha-amylase is starch
The 5%~10% of quality, the alpha-amylase are high temperature resistant enzyme.
Preferably, in step (1), described to be adjusted to pH value of solution be 4.5~6.5 is adjusted by the way that hydrochloric acid is added.
Preferably, in step (1), the enzyme deactivation is by being heated rapidly to 100~120 DEG C of realizations.
Preferably, in step (2), the additional amount of the mixed enzyme is the 0.5%~3% of step (2) starch quality；Institute
The pH for the sodium-acetate buffer stated is 5~6.5；The starch milk mass concentration is 30%~45%.
Preferably, in step (2), described to be adjusted to pH be 7~8 is NaOH solution by the way that 0.5~1.5mol/L is added
It adjusts.
Preferably, in step (3), the maltodextrin and porous-starch mass ratio are 0.5:1~2:1；Described is mixed
Close 20~40wt% of concentration of liquid；The crosslinking agent additional amount is the 0.01~0.1% of porous-starch quality.
Preferably, in step (3), the adjusting pH of mixed to 7~8 is realized by the way that HCl solution is added.
Preferably, in step (4), mass ratio 1:1~1:3 of the soluble perfume and essence wall material；Described is equal
Matter is carried out by homogenizer；The revolving speed of homogenizer is 12000~20000r/min, and the time of homogeneous is 15~30min；
The soluble perfume is one of lemon extract, grapefruit essence and flavoring orange essence or a variety of.
A kind of high embedding essence microcapsule, is made by above-mentioned preparation method, and the embedding rate of essence is 85%~100%；
Peroxide value after 60 DEG C of gained microcapsules oxidation 12d is lower than 0.15g/100g.The essence microcapsule is environmentally protective, embeddability properties
Well, oxidation resistance is strong, and essence stability can be improved.
Compared with prior art, the present invention has the advantage that
(1) wall material raw material of the invention have apparent antioxidation to essence.Porous-starch uses complex enzyme legal system
Standby, surface to inside has compared with multiple hole, and huge specific surface area assigns its excellent physical absorption ability, can be adsorbed on essence
Inside wall material, thin film can be formed on starch surface after the molten water of maltodextrin, be conducive to completely cut off light, heat, oxygen etc., so
Essence good in oxidation resistance after embedding.It is compared with the essence not embedded, by taking lemon as an example, after 60 DEG C of oxidation 12d,
The lemon peroxide value not embedded is 0.7133g/100g, and the peroxide value (POV) of the lemon after embedding is only
0.135g/100g。
(2) compared with existing Micro-Encapsulation Technique, the present invention using maltodextrin and porous-starch cross-linking products as
Wall material can further improve the embedding rate and inoxidizability of starch.Cross-linking reaction makes porous-starch molecule, maltodextrin molecule
In the molecule or it is intermolecular react, form a kind of tridimensional network, on the one hand this tridimensional network can enhance shallow lake
The adsorptivity of powder enhances the adsorption capacity to essence, on the other hand porous-starch and maltodextrin can be made to link together, made micro-
Capsule wall material structure is finer and close, improves embeddability properties, delays to aoxidize.With non-crosslinked, directly embedding after wall material is simply mixed
Essence comparison, by taking lemon as an example, it is 62.35% that the essence microcapsule embedding rate that directly embeds afterwards, which is simply mixed, in wall material,
It and is 87.36% by the essence microcapsule embedding rate embedded after wall material crosslinking；After 60 DEG C of oxidation 12d, wall material is simply mixed
The essence microcapsule peroxide value directly embedded afterwards is 0.3879g/100g, and the essence microcapsule mistake that will be embedded after wall material crosslinking
Oxidation number is only 0.135g/100g.
(3) present invention process is simple, using starch as chief component, have edible, high efficiency, high value, it is low at
This characteristics of.
(4) used wall material is mostly simple mixing in the patent at present, and the technology of the present invention is using chemical reagent crosslinking
Method will embed again after wall material crosslinking, and compared with technology before, the embedding rate of essence is improved, antioxygenic property enhancing.
Specific embodiment
Below with reference to reality, by example is applied, the present invention is further illustrated, but the scope of protection of present invention is not limited to
In the range of embodiment statement.
The measuring method of essence microcapsule embedding rate obtained in the embodiment of the present invention is as follows:
With reference to bright red plum etc., (bright red plum, Zhang Yanjun, Xu Fei wait the preparation of .4 kind physical method fragrant to the measuring method of embedding rate
Comparative analysis [J] Food Science of cymbidium essential oil microcapsules, 2017,38 (21): 106-111.) method.Embedding rate is to measure
Embedded samples embed an important indicator of effect, are the ratios for embedding content (total oil removes surface oil) total oil content of Zhan of grease
Weight.Fuel load, that is, embedded samples absorption grease total content, i.e., total oil content.
The measurement of surface oil content: essence microcapsule (m) obtained in 5g embodiment is taken to extract in 60mL petroleum ether
10min is filtered with G3 sand core funnel, filter residue 10mL petroleum ether immediately.Filtrate is shifted to known quality (m1) suction filtration
In bottle, rotated under conditions of 40 DEG C to constant weight (m with Rotary Evaporators2).Calculating is shown below.
Surface oil content (%)=(m2-m1)/m × 100%
The measurement of total oil content: the total oil content of embedded samples is measured using alkaline ether method.It takes obtained in 5g embodiment
Essence microcapsule (m3) in separatory funnel, 60 DEG C of water of 10mL are added and shake up, dissolve it sufficiently.It is dense to sequentially add 1.25mL
Ammonium hydroxide, 10mL dehydrated alcohol, shakes up.25mL anhydrous ether is added, opens plug deflation after shaking 1min.25mL petroleum ether is added,
Shaking mixes, and opening plug and standing makes its layering.Supernatant liquor is collected in the bottle,suction (m of known quality4) in, existed with Rotary Evaporators
It rotates under conditions of 40 DEG C to constant weight (m5).Calculation formula is shown below.
Total oil content (%)=(m5-m4)/m3× 100%
The measurement of embedding rate: the content of the content of embedding rate surface oil and total oil indicates that calculation formula is shown below.
Embedding rate (%)=(total oil content-surface oil content)/total oil content × 100%
The measuring method of essence antioxygenic property measurement experiment method obtained in the embodiment of the present invention is as follows:
Referring to Wu Kegang etc., (Wu Kegang, Meng Hongchang utilize converted starch microencapsulation to antioxygenic property measurement experiment method
Research [J] Food Science of the unicellular DHA grease of microalgae, 2004 (07): 75-78.) method.By the microcapsules in embodiment
Sample is placed under conditions of 60 DEG C, carries out accelerated oxidation test, is taken out in the 2 day time of preset interval, first will be in embodiment
Microcapsules sample total oil is extracted using alkaline ether method, method with total oil content measurement, further according to " GB 5009.227-
The measurement of peroxide value in 2016 national food safety standard food ", its peroxide value (POV) is measured, cycle set is 12 days.
Comparative example 1
Wall is used as after two kinds of wall material raw material (porous-starch and maltodextrin) are simply mixed in proportion by the prior art
Material, lemon are added after emulsifier homogeneous and are sent into spray drying in spray dryer and obtain microcapsule product as core material.
After tested, total oil content obtained by the present embodiment be 43.28%, surface oil content 16.29%, embedding rate is
62.35%；；After 60 DEG C of oxidation 12d, essence microcapsule lemon peroxide value is 0.3879g/100g.
Embodiment 1
50g cornstarch adds water to be made into 30% starch milk, and hydrochloric acid solution is adjusted to pH value of solution 4.5, starchiness is added
The alpha-amylase of amount 5% reduces temperature to 60 DEG C after 85 DEG C of holding 20min, continues conversion to DE to 11, is heated rapidly to
100 DEG C of enzyme deactivations stop conversion.It is spray-dried that white fine powder is made, obtain maltodextrin.
The starch milk that 50g cornstarch is made into 30% with sodium-acetate buffer (pH=5) is weighed, in 50 DEG C of stirred in water bath
After mixing preheating, the mixed enzyme (alpha-amylase: amyloglucosidase of 0.5% (starch quality/mixed enzyme volume, w/v) is added
=1:1, volume ratio) reaction 6h after, be adjusted to pH=7 with the NaOH solution of 0.5mol/L.Washing, dry, sieving obtains porous shallow lake
Powder.
It is 0.5:1 with mass ratio, maltodextrin is mixed with porous-starch；Addition distilled water, which is stirred, is made into 20%
Crosslinking agent sodium trimetaphosphate is added with the ratio that the mass ratio of crosslinking agent and porous-starch is 0.01% in the solution of (mass ratio),
PH of mixed is adjusted to 9 using NaOH solution, is put into 30 DEG C of waters pot and is stirred, after stirring 4h, is adjusted using HCl solution mixed
Conjunction liquid pH to 7 obtains essence wall material after washing, dry, crushing and sieving.
It takes essence wall material that the solution that distilled water is made into 20% is added, adds 0.5% emulsifier dodecyl benzene sulfonic acid
Sodium, suitably heating stirring dissolves it sufficiently in water bath with thermostatic control, is cooled to room temperature.By lemon extract (core wall ratio, i.e. essence with
The mass ratio of essence wall material is 1:1) it is slowly added in the wall material solution prepared, with high speed disperser in 12000r/min,
The matter time is uniformly dispersed under conditions of being 30min, and homogeneous forms uniform emulsion, and solid-state flowing can be obtained by carrying out spray drying
The powder microcapsule essence product of property.
After tested, total oil content obtained by the present embodiment be 57.80%, surface oil content 7.30%, embedding rate is
87.36%；After 60 DEG C of oxidation 12d, essence microcapsule lemon peroxide value is 0.135g/100g.
Compared with comparative example 1, the embedding rate of essence microcapsule product obtained by this method is higher, aoxidizes by 60 DEG C
Peroxide value is lower after 12d, i.e., oxidation resistance improves.It is primarily due to make the cross-linking products of maltodextrin and porous-starch
It can further improve the embedding rate and inoxidizability of starch for wall material.Cross-linking reaction makes porous-starch molecule, maltodextrin point
Son in the molecule or it is intermolecular react, form a kind of tridimensional network, on the one hand this tridimensional network can enhance
The adsorptivity of starch enhances the adsorption capacity to essence, on the other hand porous-starch and maltodextrin can be made to link together, made
Microcapsule wall material structure is finer and close, improves embeddability properties, delays to aoxidize.
Embodiment 2
100g potato starch adds water to be made into 35% starch milk, and hydrochloric acid solution is adjusted to pH value of solution=6.5, is added and forms sediment
The alpha-amylase of silty amount 6% reduces temperature to 75 DEG C after 85 DEG C of holding 30min, continues conversion to DE to 11, quickly adds
Heat stops conversion to 110 DEG C of enzyme deactivations.It is spray-dried that white fine powder is made, obtain maltodextrin.
The starch milk that 100g potato starch is made into 40% with sodium-acetate buffer (pH=5.5) is weighed, in 50 DEG C of water-baths
In stir and evenly mix preheating after, be added starch quality 1% mixed enzyme (alpha-amylase: amyloglucosidase=1.5:1).Reaction
After 9h, pH=8 is adjusted to the NaOH solution of 1mol/L.Washing, dry, sieving obtains porous-starch.
It is 1:1 with mass ratio, maltodextrin is mixed with porous-starch；Addition distilled water, which is stirred, is made into 30% (quality
Than) solution, the ratio that the mass ratio of crosslinking agent and porous-starch is 0.02% is added crosslinking agent phosphorus oxychloride, uses NaOH solution
PH of mixed is adjusted to 9.5, is put into 40 DEG C of waters pot and stirs, after stirring 8h, adjust pH of mixed to 7 with HCl solution, wash
Essence wall material is obtained after washing, dry, crush and being sieved.
It takes essence wall material that the solution that distilled water is made into 30% is added, adds 1% emulsifier neopelex,
Suitably heating stirring dissolves it sufficiently in water bath with thermostatic control, is cooled to room temperature.By orange flavor (core wall ratio, i.e. essence and perfume
The mass ratio of smart wall material is 1:2) it is slowly added in the wall material solution prepared, with high speed disperser in 15000r/min, homogeneous
Time is uniformly dispersed under conditions of being 20min, and homogeneous forms uniform emulsion, and solid-state mobility can be obtained by carrying out spray drying
Powder microcapsule essence product.
Embedding is the results showed that reached 88.51% using the embedding rate of wall material embedding orange flavor of the invention, warp
After crossing 60 DEG C of oxidation 12d, the peroxide value of pure orange flavor is 0.7133g/100g.
Embodiment 3
150g pea starch adds water to be made into 35% starch milk, and hydrochloric acid solution is adjusted to pH value of solution=6.5, starch is added
The alpha-amylase of quality 7% reduces temperature to 75 DEG C after 85 DEG C of holding 40min, continues conversion to DE to 12, quickly heats
To 120 DEG C of enzyme deactivations, stop conversion.It is spray-dried that white fine powder is made, obtain maltodextrin.
The starch milk that 150g pea starch is made into 45% with sodium-acetate buffer (pH=5.5) is weighed, in 50 DEG C of water-baths
After stirring and evenly mixing preheating, the mixed enzyme (alpha-amylase: amyloglucosidase=1.5:1) of starch quality 1.5% is added.Reaction
After 12h, pH=7 is adjusted to the NaOH solution of 1mol/L.Washing, dry, sieving obtains porous-starch.
It is 0.5:1 with mass ratio, maltodextrin is mixed with porous-starch；It a certain amount of distilled water is added is stirred and be made into
Crosslinking agent epoxychloropropane is added in the ratio that the mass ratio of 30% solution, crosslinking agent and porous-starch is 0.04%, uses NaOH
Solution adjusts pH of mixed to 10, is put into 40 DEG C of waters pot and stirs, after stirring 12h, with HCl solution adjust pH of mixed to
7, essence wall material is obtained after washing, dry, crushing and sieving.
It takes essence wall material that the solution that distilled water is made into 40% is added, 2% emulsifier alkylbenzene naphthenic acid sodium is added, in perseverance
Suitably heating stirring dissolves it sufficiently in tepidarium, is cooled to room temperature.By grapefruit essence (core wall ratio, i.e. essence and essence wall
The mass ratio of material is 1:3) it is slowly added in the wall material solution prepared, with high speed disperser in 20000r/min, homogenizing time
To be uniformly dispersed under conditions of 30min, homogeneous forms uniform emulsion, and the powder of solid-state mobility can be obtained by carrying out spray drying
Last microcapsule essence product.
Embedding is the results showed that reached 89.32% using the embedding rate of wall material embedding grapefruit essence of the invention, warp
After crossing 60 DEG C of oxidation 12d, the peroxide value of pure grapefruit essence is 0.7133g/100g.
Embodiment 4
250g tapioca adds water to be made into 40% starch milk, and hydrochloric acid solution is adjusted to pH value of solution=5, starchiness is added
The alpha-amylase of amount 8% reduces temperature to 75 DEG C after 90 DEG C of holding 50min, continues conversion to DE to 13, is heated rapidly to
120 DEG C of enzyme deactivations stop conversion.It is spray-dried that white fine powder is made, obtain maltodextrin.
The starch milk that 250g tapioca is made into 30% with sodium-acetate buffer (pH=6.5) is weighed, in 50 DEG C of water-baths
After stirring and evenly mixing preheating, the mixed enzyme (alpha-amylase: amyloglucosidase=2:1) of starch quality 2% is added.React 15h
Afterwards, pH=8 is adjusted to the NaOH solution of 1.5mol/L.Washing, dry, sieving obtains porous-starch.
It is 0.5:1 with mass ratio, maltodextrin is mixed with porous-starch；It a certain amount of distilled water is added is stirred and be made into
Crosslinking agent phosphorus oxychloride is added in the ratio that the mass ratio of 30% solution, crosslinking agent and porous-starch is 0.06%, utilizes NaOH
Solution adjusts pH of mixed to 10, is put into 40 DEG C of waters pot and stirs, after stirring 12h, adjusts pH of mixed using HCl solution
To 7, essence wall material is obtained after washing, dry, crushing and sieving.
It takes essence wall material that the solution that distilled water is made into 30% is added, adds 1.5% emulsifier dodecyl benzene sulfonic acid
Sodium, suitably heating stirring dissolves it sufficiently in water bath with thermostatic control, is cooled to room temperature.By vanilla (core wall ratio, i.e. essence with
The mass ratio of essence wall material is 1:3) it is slowly added in the wall material solution prepared, with high speed disperser in 18000r/min,
The matter time is uniformly dispersed under conditions of being 25min, and homogeneous forms uniform emulsion, and solid-state flowing can be obtained by carrying out spray drying
The powder microcapsule essence product of property.
Embedding is the results showed that reached 89.32% using the embedding rate of wall material embedding vanilla of the invention, warp
After crossing 60 DEG C of oxidation 12d, the peroxide value of pure vanilla is 0.7133g/100g.
Embodiment 5
250g waxy corn starch adds water to be made into 45% starch milk, and hydrochloric acid solution is adjusted to pH value of solution=6, is added and forms sediment
The alpha-amylase of silty amount 9% reduces temperature to 70 DEG C after 85 DEG C of holding 60min, continues conversion to DE to 14, quickly adds
Heat stops conversion to 120 DEG C of enzyme deactivations.It is spray-dried that white fine powder is made, obtain maltodextrin.
The starch milk that 250g waxy corn starch is made into 30% with sodium-acetate buffer (pH=5.5) is weighed, in 50 DEG C of water
After stirring and evenly mixing preheating in bath, the mixed enzyme (alpha-amylase: amyloglucosidase=2.5:1) of starch quality 2.5% is added.
After reacting 8h, pH=7 is adjusted to the NaOH solution of 1mol/L.Washing, dry, sieving obtains porous-starch.
It is 0.5:1 with mass ratio, maltodextrin is mixed with porous-starch；It a certain amount of distilled water is added is stirred and be made into
Crosslinking agent phosphorus oxychloride and epoxy chloropropionate is added in the ratio that the mass ratio of 30% solution, crosslinking agent and porous-starch is 0.08%
Alkane (mass ratio 1:1) is put into 40 DEG C of waters pot and stirs using NaOH solution adjusting pH of mixed to 11, after stirring 16h,
Using HCl solution adjusting pH of mixed to 7, essence wall material is obtained after washing, dry, crushing and sieving.
It takes essence wall material that the solution that distilled water is made into 40% is added, adds 2% emulsifier neopelex,
Suitably heating stirring dissolves it sufficiently in water bath with thermostatic control, is cooled to room temperature.By milk flavour (core wall ratio, i.e. essence and perfume
The mass ratio of smart wall material is 1:3) it is slowly added in the wall material solution prepared, with high speed disperser in 15000r/min, homogeneous
Time is uniformly dispersed under conditions of being 20min, and homogeneous forms uniform emulsion, and solid-state mobility can be obtained by carrying out spray drying
Powder microcapsule essence product.
Embedding is the results showed that reached 90.51% using the embedding rate of wall material embedding milk flavour of the invention, warp
After crossing 60 DEG C of oxidation 12d, the peroxide value of plain chocolate essence is 0.7133g/100g.
Embodiment 6
300g rice starch adds water to be made into 35% starch milk, and hydrochloric acid solution is adjusted to pH value of solution 6.5, starchiness is added
The alpha-amylase of amount 10% reduces temperature to 75 DEG C after 85 DEG C of holding 70min, continues conversion to DE to 15, is heated rapidly to
120 DEG C of enzyme deactivations stop conversion.It is spray-dried that white fine powder is made, obtain maltodextrin.
The starch milk that 300g rice starch is made into 35% with sodium-acetate buffer (pH=6) is weighed, is stirred in 50 DEG C of water-baths
After mixing mixing preheating, the mixed enzyme (alpha-amylase: amyloglucosidase=3:1) of starch quality 3% is added.After reacting 18h,
PH=7 is adjusted to the NaOH solution of 1mol/L.Washing, dry, sieving obtains porous-starch.
It is 0.5:1 with mass ratio, maltodextrin is mixed with porous-starch；It a certain amount of distilled water is added is stirred and be made into
Crosslinking agent sodium trimetaphosphate is added in the ratio that the mass ratio of 30% solution, crosslinking agent and porous-starch is 0.1%, utilizes NaOH
Solution adjusts pH of mixed to 11, is put into 40 DEG C of waters pot and stirs, after stirring 20h, adjusts pH of mixed using HCl solution
To 7, essence wall material is obtained after washing, dry, crushing and sieving.
It takes essence wall material that the solution that distilled water is made into 35% is added, adds 1.5% emulsifier alkylbenzene naphthenic acid sodium,
Suitably heating stirring dissolves it sufficiently in water bath with thermostatic control, is cooled to room temperature.By flavoring orange essence (core wall ratio, i.e. essence and essence
The mass ratio of wall material is 1:1.5) it is slowly added in the wall material solution prepared, with high speed disperser in 19000r/min, homogeneous
Time is uniformly dispersed under conditions of being 20min, and homogeneous forms uniform emulsion, and solid-state mobility can be obtained by carrying out spray drying
Powder microcapsule essence product.
Embedding is the results showed that reached 92.22% using the embedding rate of wall material embedding flavoring orange essence of the invention, warp
After crossing 60 DEG C of oxidation 12d, the peroxide value of pure flavoring orange essence is 0.7133g/100g.
Embodiment 7
300g sweet potato starch adds water to be made into 35% starch milk, and hydrochloric acid solution is adjusted to pH value of solution 6.5, starchiness is added
The alpha-amylase of amount 6% reduces temperature to 75 DEG C after 85 DEG C of holding 80min, continues conversion to DE to 16, is heated rapidly to
110 DEG C of enzyme deactivations stop conversion.It is spray-dried that white fine powder is made, obtain maltodextrin.
The starch milk that 300g sweet potato starch is made into 45% with sodium-acetate buffer (pH=6.5) is weighed, in 50 DEG C of water-baths
After stirring and evenly mixing preheating, the mixed enzyme (alpha-amylase: amyloglucosidase=2:1) of starch quality 3% is added.React 21h
Afterwards, pH=8 is adjusted to the NaOH solution of 1.5mol/L.Washing, dry, sieving obtains porous-starch.
It is 0.5:1 with mass ratio, maltodextrin is mixed with porous-starch；It a certain amount of distilled water is added is stirred and be made into
Crosslinking agent epoxychloropropane is added in the ratio that the mass ratio of 30% solution, crosslinking agent and porous-starch is 0.0.3%, utilizes
NaOH solution adjusts pH of mixed to 10, is put into 40 DEG C of waters pot and stirs, after stirring for 24 hours, is adjusted and mixed using HCl solution
Liquid pH to 7 obtains essence wall material after washing, dry, crushing and sieving.
Spray drying experiment condition: it takes soluble perfume wall material that the solution that distilled water is made into 35% is added, adds 1%
Emulsifier neopelex, suitably heating stirring dissolves it sufficiently in water bath with thermostatic control, is cooled to room temperature.By fingered citron
(core wall ratio, i.e. essence and the mass ratio of essence wall material are slowly added in the wall material solution prepared mandarin orange essence for 1:3), with high speed
Dispersion machine is in 20000r/min, and homogenizing time is uniformly dispersed under conditions of being 30min, and homogeneous forms uniform emulsion, carries out
Spray drying can obtain the powder microcapsule essence product of solid-state mobility.
Embedding the results showed that reached 90.15% using the embedding rate of wall material embedding bergamot essence of the invention,
After 60 DEG C of oxidation 12d, the peroxide value of pure bergamot essence is 0.7133g/100g.
The present invention is not constrained by above-described embodiment, and others are any to be made without departing from the spirit and principles of the present invention
Changes, modifications, substitutions, combinations, simplifications, should be equivalent alternative, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of high embedding essence microcapsule, it is characterised in that the following steps are included:
(1) preparation of maltodextrin: starch adds water to be made into the starch milk of 30%~45% mass fraction, and being adjusted to pH value of solution is 4.5
~6.5, alpha-amylase is added, after 70~90 DEG C of 20~60min of holding, reduces temperature to 60~75 DEG C, continues conversion to DE
For value to 11~17, enzyme deactivation stops conversion；It is spray-dried that white fine powder is made, obtain maltodextrin；
(2) preparation of porous-starch: being made into starch milk with sodium-acetate buffer for starch, mixes in 45~60 DEG C of stirred in water bath
After preheating, be added mixed enzyme, reaction 6~for 24 hours after, be adjusted to pH be 7~8；Washing, dry, sieving obtains porous-starch；Described
Mixed enzyme is mixed by 1:1~3:1 mass ratio with amyloglucosidase by alpha-amylase and is formed；
(3) preparation of essence wall material: maltodextrin is mixed with porous-starch；Addition distilled water, which is stirred, is made into mixed liquor,
Crosslinking agent is added, adjust pH of mixed be 9~11,30~60 DEG C be stirred to react the time be 4~for 24 hours, adjusting pH of mixed to 7~
8, essence wall material is obtained after washing, dry, crushing, sieving；The crosslinking agent is sodium trimetaphosphate, phosphorus oxychloride and epoxy chloropropionate
One of alkane is a variety of；
(4) it the preparation of essence microcapsule: takes essence wall material that the solution that distilled water is made into 20~40% is added, adds 0.5~2%
Emulsifier heat up in water bath with thermostatic control stirring dissolve it sufficiently, be cooled to room temperature, obtain wall material solution；By soluble perfume plus
Into wall material solution, homogeneous forms uniform emulsion, and spray drying obtains the micro- glue of powdery, water-soluble essence of solid-state mobility
Capsule；The emulsifier is one or more in neopelex, neopelex and alkylbenzene naphthenic acid sodium.
2. the preparation method of high embedding essence microcapsule according to claim 1, it is characterised in that: described in step (1)
Alpha-amylase additional amount be starch quality 5%~10%, the alpha-amylase be high temperature resistant enzyme.
3. the preparation method of high embedding essence microcapsule according to claim 1, it is characterised in that: described in step (1)
Be adjusted to pH value of solution be 4.5~6.5 be by be added hydrochloric acid adjust.
4. the preparation method of high embedding essence microcapsule according to claim 1, it is characterised in that: described in step (1)
Enzyme deactivation be by being heated rapidly to 100~120 DEG C of realizations.
5. the preparation method of high embedding essence microcapsule according to claim 1, it is characterised in that: described in step (2)
Mixed enzyme additional amount be step (2) starch quality 0.5%~3%；The pH of the sodium-acetate buffer is 5~6.5；
The starch milk mass concentration is 30%~45%.
6. the preparation method of high embedding essence microcapsule according to claim 1, it is characterised in that: described in step (2)
Be adjusted to pH be 7~8 be by be added 0.5~1.5mol/L NaOH solution adjust.
7. the preparation method of high embedding essence microcapsule according to claim 1, it is characterised in that: described in step (3)
Maltodextrin and porous-starch mass ratio be 0.5:1~2:1；20~40wt% of concentration of the mixed liquor；The friendship
Join 0.01~0.1% that agent additional amount is porous-starch quality.
8. the preparation method of high embedding essence microcapsule according to claim 1, it is characterised in that: described in step (3)
Adjusting pH of mixed to 7~8 be by be added HCl solution realize.
9. the preparation method of high embedding essence microcapsule according to claim 1, it is characterised in that: described in step (4)
Soluble perfume and essence wall material mass ratio 1:1~1:3；The homogeneous is carried out by homogenizer；Homogenizer
Revolving speed be 12000~20000r/min, time of homogeneous is 15~30min；The soluble perfume is lemon extract, west
One of shaddock flavor essence and flavoring orange essence are a variety of.
10. a kind of high embedding essence microcapsule, which is characterized in that it is by the described in any item preparation method systems of claim 1-9
, the embedding rate of essence is 85%~100%, and the peroxide value after 60 DEG C of gained water soluble microcapsule oxidation 12d is lower than
0.15g/100g。
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| CN114304584A (en) * | 2021-12-28 | 2022-04-12 | 广州昆特臣香精香料科技有限公司 | Preparation method of essence microcapsule and essence microcapsule |
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