CN110214919B - High-embedding essence microcapsule and preparation method thereof - Google Patents

High-embedding essence microcapsule and preparation method thereof Download PDF

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CN110214919B
CN110214919B CN201910605711.4A CN201910605711A CN110214919B CN 110214919 B CN110214919 B CN 110214919B CN 201910605711 A CN201910605711 A CN 201910605711A CN 110214919 B CN110214919 B CN 110214919B
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essence
solution
starch
microcapsule
wall material
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CN110214919A (en
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高群玉
戴桂芳
陈云
陈小玲
辛少平
徐咪
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I&D INTERNATIONAL FLAVOURS & FRAGRANCES (GZ) CO LTD
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I&D INTERNATIONAL FLAVOURS & FRAGRANCES (GZ) CO LTD
South China University of Technology SCUT
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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
    • 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
    • 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

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Nutrition Science (AREA)
  • Molecular Biology (AREA)
  • Seasonings (AREA)
  • Cosmetics (AREA)
  • Manufacturing Of Micro-Capsules (AREA)
  • General Preparation And Processing Of Foods (AREA)

Abstract

The invention discloses a high-embedding essence microcapsule and a preparation method thereof. The preparation method comprises mixing maltodextrin and porous starch; adding distilled water, stirring and mixing to prepare a mixed solution, adding a cross-linking agent, adjusting the pH of the mixed solution to 9-11, stirring and reacting at 30-60 ℃ for 4-24 hours, adjusting the pH of the mixed solution to 7-8, washing, drying, crushing and sieving to obtain an essence wall material; adding essence into the wall material solution, homogenizing to form uniform emulsion, and spray drying to obtain essence microcapsule. The product of the invention is green and environment-friendly, the cost is low, the embedding rate of the essence after the microcapsule is adsorbed is higher than 85%, and the peroxide value after the microcapsule is oxidized for 12 days at 60 ℃ is lower than 0.15g/100g. The method can improve the embedding rate of the essence, delay the oxidation of the essence, and is beneficial to the storage, transportation, application and popularization of the essence.

Description

High-embedding essence microcapsule and preparation method thereof
Technical Field
The invention relates to the technical field of essence and spice treatment, in particular to a high-embedding essence microcapsule and a preparation method thereof.
Background
The edible essence refers to a fragrant substance which has the fragrance of natural melons and fruits and can be eaten, and the edible essence can endow fragrance to food raw materials, makes up the deficiency of the fragrance in food, improves and optimizes the flavor of the food, and is widely applied to the modern food industry. The essence can be divided into top note, body note and base note according to the sense of olfactory organ. The water-soluble essence is prepared by blending natural perfume and synthetic perfume, and dissolving with ethanol water solution (or other water-soluble solvents such as propylene glycol), and is mainly used for soft beverage, wine, etc.
The common essences are mostly composed of substances such as alcohol, aldehyde, ketone, acid, ester and the like, the substances have lower boiling points, and many substances contain unsaturated bonds, so that the substances are sensitive to damp heat, easy to volatilize, easy to oxidize, easy to react with other components and the like, loss in the food processing and storage processes often occurs, and the substances can be well protected by adopting a modern technology, so that the stability and the processability of the substances are improved. The microcapsule technology is a common method for embedding essence, and microencapsulation treatment is beneficial to improving the stability of the essence. The materials which can be used as the wall materials of the microcapsules are many, and the commonly used wall materials can be classified into carbohydrates such as starch, starch syrup dry powder, maltodextrin, chitosan, small molecular saccharides, sodium alginate and various plant gums (Arabic gum, carrageenan, xanthan gum, pectin and the like) according to the chemical properties of the wall materials; proteins such as soy protein, gelatin, zein, whey protein, etc.; waxes and lipids such as beeswax, paraffin, grease, liposomes, etc. In recent years, many patents and articles for embedding essence in various microcapsule wall materials are reported, and mainly focus on improving the slow release type and embedding rate of the essence.
Chinese invention patent 2011104404693 discloses a microcapsule prepared by taking Arabic gum and beta-cyclodextrin or Arabic gum maltodextrin or Arabic gum porous starch as wall material solution, taking blackberry anthocyanin extract as core material, adding an anticaking agent and then carrying out spray drying; chinese invention patent application 2014107000553 discloses a microcapsule prepared from 10-20% of oviductus ranae polypeptide core materials, 30-50% of maltodextrin, 10-20% of sodium carboxymethyl cellulose, 5-20% of beta-cyclodextrin and 5-10% of porous starch. However, the core material embedding rate of the technology needs to be further improved, and the technology mainly adopts embedding to protect the core material, although the core material is beneficial to avoiding the direct contact of the core material with the outside and has certain protection on the contact with oxygen, the performance characteristics of the wall material, such as the comprehensive performance of heat insulation, light shielding and oxygen isolation of the wall material, are not considered, and the protection of the core material sensitive to light, heat and oxygen is limited.
Disclosure of Invention
The invention aims to solve the technical problem of providing an essence microcapsule which has better protection on light, heat and oxygen and high embedding rate and a preparation method thereof, the prepared essence microcapsule product is green and environment-friendly, the cost is low, the essence embedding rate of the essence microcapsule is higher than 85%, and the peroxide value after being oxidized for 12 days at 60 ℃ is lower than 0.15g/100g.
The invention takes renewable resource starch as raw material, and can adopt various different starches, such as corn starch, waxy corn starch, potato starch, pea starch, rice starch and the like. The maltodextrin and the porous starch are prepared by different enzymolysis of starch. Since both maltodextrin and porous starch have hydroxyl groups, a substance having a di-or poly-functional group (crosslinking agent) can react with maltodextrin and porous starch. The cross-linking reaction enables the porous starch molecules and the maltodextrin molecules to react in molecules or between molecules to form a three-dimensional network structure, and the three-dimensional network structure can enhance the adsorption of the starch on one hand and can connect the porous starch and the maltodextrin on the other hand, so that the embedding performance of a mixture obtained by the reaction is improved. The emulsifier is added into the core material and the wall material, and the emulsifier is favorable for forming uniform emulsion by different composition components in the core material and the wall material due to good hydrophily and lipophilicity, is favorable for protecting essence during spray drying, can effectively avoid the volatilization and oxidation of the essence at high temperature, and improves the embedding rate of the microcapsule.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a high-embedding essence microcapsule comprises the following steps:
(1) Preparation of maltodextrin: adding water into starch to prepare 30-45 mass percent of starch milk, adjusting the pH value of the solution to 4.5-6.5, adding alpha-amylase, keeping the solution at 70-90 ℃ for 20-60 min, reducing the temperature to 60-75 ℃, continuing to convert the solution to a DE value of 11-17, inactivating the enzyme, and stopping converting; spray drying to obtain white fine powder to obtain maltodextrin;
(2) Preparing porous starch: preparing starch into starch milk by using a sodium acetate buffer solution, uniformly stirring and preheating in a water bath at 45-60 ℃, adding mixed enzyme, reacting for 6-24 hours, and adjusting the pH value to 7-8; washing, drying and sieving to obtain porous starch; the mixed enzyme is formed by mixing alpha-amylase and amyloglucosidase according to the mass ratio of 1-3;
(3) Preparing essence wall materials: mixing maltodextrin with porous starch; adding distilled water, stirring and mixing to prepare a mixed solution, adding a cross-linking agent, adjusting the pH of the mixed solution to 9-11, stirring and reacting at 30-60 ℃ for 4-24 hours, adjusting the pH of the mixed solution to 7-8, washing, drying, crushing and sieving to obtain an essence wall material; the cross-linking agent is one or more of sodium trimetaphosphate, phosphorus oxychloride and epichlorohydrin;
(4) Preparing essence microcapsules: adding distilled water into essence wall material to prepare 20-40% solution, adding 0.5-2% emulsifier, heating and stirring in constant temperature water bath to dissolve completely, and cooling to room temperature to obtain wall material solution; adding water-soluble essence into the wall material solution, homogenizing to form uniform emulsion, and spray drying to obtain solid flowable powdery water-soluble essence microcapsule; the emulsifier is one or more of sodium dodecyl benzene sulfonate, sodium dodecyl benzene sulfonate and sodium alkyl benzene sulfonate.
In order to further achieve the object of the present invention, preferably, in the step (1), the amount of the α -amylase added is 5% to 10% of the mass of the starch, and the α -amylase is a thermostable enzyme.
Preferably, in the step (1), the pH value of the solution is adjusted to 4.5-6.5 by adding hydrochloric acid.
Preferably, in step (1), the enzyme deactivation is realized by rapidly heating to 100-120 ℃.
Preferably, in the step (2), the adding amount of the mixed enzyme is 0.5-3% of the mass of the starch in the step (2); the pH value of the sodium acetate buffer solution is 5-6.5; the mass concentration of the starch milk is 30-45%.
Preferably, in the step (2), the pH value is adjusted to 7-8 by adding 0.5-1.5 mol/L NaOH solution.
Preferably, in the step (3), the mass ratio of the maltodextrin to the porous starch is 0.5; the concentration of the mixed solution is 20-40 wt%; the addition amount of the cross-linking agent is 0.01-0.1% of the mass of the porous starch.
Preferably, in the step (3), the pH of the mixed solution is adjusted to 7-8 by adding HCl solution.
Preferably, in the step (4), the mass ratio of the water-soluble essence to the essence wall material is 1; the homogenization is carried out by stirring through a homogenizer; the rotating speed of the homogenizer is 12000-20000 r/min, and the homogenizing time is 15-30 min; the water-soluble essence is one or more of lemon essence, grapefruit essence and orange essence.
A high-embedding essence microcapsule is prepared by the preparation method, and the embedding rate of the essence is 85-100%; the peroxide value of the obtained microcapsule after being oxidized for 12 days at 60 ℃ is lower than 0.15g/100g. The essence microcapsule is environment-friendly, has good embedding property and strong oxidation resistance, and can improve essence stability.
Compared with the prior art, the invention has the following advantages:
(1) The wall material raw material of the invention has obvious antioxidation on the essence. The porous starch is prepared by adopting a compound enzyme method, a plurality of holes are formed from the surface to the inside, the huge specific surface area endows the porous starch with excellent physical adsorption capacity, the essence can be adsorbed in the wall material, a layer of film is formed on the surface of the starch after the maltodextrin dissolves water, and the light, heat, oxygen and the like can be favorably isolated, so that the oxidation resistance of the embedded essence is good. Compared with the essence without embedding, taking the lemon essential oil as an example, after being oxidized for 12 days at 60 ℃, the peroxide value of the non-embedded lemon essential oil is 0.7133g/100g, while the peroxide value (POV) of the embedded lemon essential oil is only 0.135g/100g.
(2) Compared with the existing microcapsule preparation technology, the invention takes the cross-linked product of maltodextrin and porous starch as the wall material, which can further improve the embedding rate and the oxidation resistance of the starch. The cross-linking reaction makes porous starch molecule and maltodextrin molecule react in or among molecules to form a three-dimensional network structure, which can enhance the adsorption of starch and the adsorption capacity of essence on one hand, and can connect porous starch and maltodextrin on the other hand, so that the wall structure of the microcapsule is more compact, the embedding performance is improved, and the oxidation is delayed. Compared with the essence which is not crosslinked and is directly embedded after the wall material is simply mixed, taking the lemon essential oil as an example, the embedding rate of the essence microcapsule which is directly embedded after the wall material is simply mixed is 62.35 percent, and the embedding rate of the essence microcapsule which is embedded after the wall material is crosslinked is 87.36 percent; after the mixture is oxidized for 12 days at the temperature of 60 ℃, the peroxide value of the directly embedded essence microcapsule after the wall materials are simply mixed is 0.3879g/100g, and the peroxide value of the embedded essence microcapsule after the wall materials are crosslinked is only 0.135g/100g.
(3) The invention has simple process, takes starch as a main component, and has the characteristics of edibility, high efficiency, high value and low cost.
(4) The wall materials used in the prior patent are mostly simply mixed, the technology of the invention adopts a chemical reagent crosslinking method to crosslink the wall materials and then embed the wall materials, and compared with the prior art, the embedding rate of the essence is improved, and the oxidation resistance is enhanced.
Detailed Description
The present invention will be further described with reference to the following examples, but the scope of the present invention is not limited to the examples.
The method for measuring the embedding rate of the essence microcapsules obtained in the embodiment of the invention comprises the following steps:
the embedding rate is measured by referring to the comparative analysis of 4 physical methods for preparing vanilla essential oil microcapsules [ J ] food science, 2017,38 (21): 106-111 ]. The embedding rate is an important index for measuring the embedding effect of an embedded sample, and is the proportion of the content of embedding grease (total oil except surface oil) to the content of the total oil. The oil loading amount is the total oil content of the embedded sample for absorbing the grease.
Measurement of surface oil content: 5G of the flavour microcapsules (m) obtained in the example were extracted in 60mL of petroleum ether for 10min, immediately filtered off with a G3 sand-core funnel and the filter residue was washed with 10mL of petroleum ether. Transfer filtrate to known mass (m) 1 ) In a rotary evaporator at 40 ℃ to constant weight (m) 2 ). The calculation is shown below.
Surface oil content (%) = (m) 2 -m 1 )/m×100％
Determination of the total oil content: the total oil content of the embedded sample is determined by adopting an alkaline ether method. 5g of the perfume microcapsules obtained in the example (m) 3 ) Then, 10mL of 60 ℃ water was added to the separatory funnel and shaken to dissolve it sufficiently. 1.25mL of concentrated ammonia water and 10mL of absolute ethyl alcohol are added in sequence and shaken up. Then 25mL of anhydrous ether is added, the mixture is shaken for 1min, and then the plug is opened to release the gas. Adding 25mL of petroleum ether, shaking and mixing uniformly, opening a plug and standing to separate the mixture into layers. The supernatant was collected in a filtration flask (m) of known mass 4 ) In the process, the mixture is subjected to rotary evaporation to constant weight (m) by a rotary evaporator at the temperature of 40 DEG C 5 ). The calculation formula is shown in the following formula.
Total oil content (%) = (m) 5 -m 4 )/m 3 ×100％
Determination of the embedding rate: the content of the embedding rate is represented by the contents of the surface oil and the total oil, and the calculation formula is shown as the following formula.
Entrapment Rate (%) = (Total oil content-surface oil content)/Total oil content × 100%
The measuring method of the experimental method for measuring the antioxidant performance of the essence obtained in the embodiment of the invention comprises the following steps:
the experimental method for measuring the antioxidant performance refers to a method of Wukegang and the like (Wukegang, membenchang. Research on microalgae single-cell DHA grease by utilizing modified starch microencapsulation [ J ]. Food science, 2004 (07): 75-78.). The microcapsule samples in the examples are placed at 60 ℃ for an accelerated oxidation test, and are taken out at preset intervals of 2 days, the total oil of the microcapsule samples in the examples is extracted by adopting an alkaline diethyl ether method, the method is the same as the determination of the content of the total oil, and the peroxide value (POV) of the microcapsule samples is determined according to the determination of the peroxide value in GB 5009.227-2016 food safety national standard food, and the period is set as 12 days.
Comparative example 1
According to the prior art, two wall material raw materials (porous starch and maltodextrin) are simply mixed according to a proportion to be used as a wall material, lemon essential oil is used as a core material, an emulsifier is added to homogenize the mixture, and the mixture is sent into a spray dryer to be spray-dried to obtain a microcapsule product.
Through tests, the total oil content obtained in the embodiment is 43.28%, the surface oil content is 16.29%, and the embedding rate is 62.35%; (ii) a After being oxidized for 12 days at the temperature of 60 ℃, the peroxide value of the essence microcapsule lemon essential oil is 0.3879g/100g.
Example 1
Adding water into 50g of corn starch to prepare 30% starch milk, adjusting the pH of the solution to 4.5 by using a hydrochloric acid solution, adding alpha-amylase accounting for 5% of the mass of the starch, keeping the temperature at 85 ℃ for 20min, reducing the temperature to 60 ℃, continuing to convert the starch to DE to 11, rapidly heating the starch to 100 ℃ to inactivate the enzyme, and stopping the conversion. Spray drying to obtain white fine powder, and obtaining the maltodextrin.
50g of corn starch is weighed and mixed with a sodium acetate buffer solution (pH = 5) to prepare 30% starch milk, the starch milk is stirred, mixed, preheated and added with 0.5% (mass of starch/volume of mixed enzyme, w/v) mixed enzyme (alpha-amylase: amyloglucosidase =1, volume ratio) to react for 6 hours, and then the mixture is adjusted to pH =7 with 0.5mol/L NaOH solution. Washing, drying and sieving to obtain porous starch.
Mixing maltodextrin and porous starch according to a mass ratio of 0.5; adding distilled water, stirring and mixing to prepare a solution of 20% (mass ratio), adding sodium trimetaphosphate serving as a crosslinking agent in a mass ratio of 0.01% of the crosslinking agent to the porous starch, adjusting the pH of the mixed solution to 9 by using a NaOH solution, stirring in a water pan at 30 ℃, adjusting the pH of the mixed solution to 7 by using an HCl solution after stirring for 4 hours, and washing, drying, crushing and sieving to obtain the essence wall material.
Adding distilled water into the essence wall material to prepare a 20% solution, adding 0.5% emulsifier sodium dodecyl benzene sulfonate, heating and stirring in a constant-temperature water bath to fully dissolve the essence wall material, and cooling to room temperature. Slowly adding lemon essence (the core-wall ratio, namely the mass ratio of the essence to the essence wall materials is 1).
Through tests, the total oil content, the surface oil content and the embedding rate of the obtained oil are respectively 57.80%, 7.30% and 87.36%; after being oxidized for 12 days at the temperature of 60 ℃, the peroxide value of the essence microcapsule lemon essential oil is 0.135g/100g.
Compared with the comparative example 1, the embedding rate of the essence microcapsule product obtained by the method is higher, and the peroxide value is lower after the product is oxidized for 12 days at 60 ℃, namely the oxidation resistance is improved. Mainly because the cross-linking product of maltodextrin and porous starch is used as a wall material to further improve the embedding rate and the oxidation resistance of the starch. The porous starch molecules and the maltodextrin molecules are subjected to intramolecular or intermolecular reaction through the crosslinking reaction to form a three-dimensional network structure, and the three-dimensional network structure can enhance the adsorbability of the starch and the adsorption capacity of the essence on one hand, and can connect the porous starch and the maltodextrin on the other hand, so that the wall material structure of the microcapsule is more compact, the embedding performance is improved, and the oxidation is delayed.
Example 2
Adding water into 100g of potato starch to prepare 35% starch milk, adjusting the pH of the solution to be =6.5 by using a hydrochloric acid solution, adding alpha-amylase accounting for 6% of the mass of the starch, keeping the solution at 85 ℃ for 30min, reducing the temperature to 75 ℃, continuing to convert the starch to DE (dextrose equivalent) to 11, rapidly heating the solution to 110 ℃ to inactivate the enzyme, and stopping the conversion. Spray drying to obtain white fine powder, and obtaining the maltodextrin.
100g of potato starch was weighed and mixed with a sodium acetate buffer (pH = 5.5) to prepare 40% starch milk, and after stirring, mixing and preheating in a water bath at 50 ℃, mixed enzyme (α -amylase: amyloglucosidase = 1.5. After 9h of reaction, the pH was adjusted to pH =8 with 1mol/L NaOH solution. Washing, drying and sieving to obtain porous starch.
Mixing maltodextrin and porous starch according to a mass ratio of 1; adding distilled water, stirring and mixing to prepare a 30% (mass ratio) solution, adding a crosslinking agent phosphorus oxychloride according to the mass ratio of the crosslinking agent to the porous starch of 0.02%, adjusting the pH of the mixed solution to 9.5 by using a NaOH solution, putting the mixed solution into a water pan at 40 ℃, stirring for 8 hours, adjusting the pH of the mixed solution to 7 by using an HCl solution, washing, drying, crushing and sieving to obtain the essence wall material.
Adding distilled water into essence wall material to prepare 30% solution, adding 1% emulsifier sodium dodecyl benzene sulfonate, heating and stirring in constant temperature water bath to dissolve completely, and cooling to room temperature. Slowly adding sweet orange essence (the core-wall ratio, namely the mass ratio of the essence to the essence wall material is 1.
The embedding experiment result shows that: the embedding rate of the sweet orange essence embedded by the wall material reaches 88.51 percent, and the peroxide value of the pure sweet orange essence is 0.7133g/100g after the pure sweet orange essence is oxidized at 60 ℃ for 12 days.
Example 3
Adding water into 150g of pea starch to prepare 35% of starch milk, adjusting the pH of the solution to be =6.5 by using a hydrochloric acid solution, adding alpha-amylase accounting for 7% of the mass of the starch, keeping the solution at 85 ℃ for 40min, reducing the temperature to 75 ℃, continuing to convert the solution to DE to 12, rapidly heating the solution to 120 ℃ to inactivate the enzyme, and stopping the conversion. Spray drying to obtain white fine powder, and obtaining the maltodextrin.
150g of pea starch was weighed and mixed with a sodium acetate buffer (pH = 5.5) to prepare a 45% starch milk, and after stirring, mixing and preheating in a water bath at 50 ℃, mixed enzyme (α -amylase: amyloglucosidase = 1.5. After 12h of reaction, the pH was adjusted to pH =7 with 1mol/L NaOH solution. Washing, drying and sieving to obtain porous starch.
Mixing maltodextrin and porous starch according to the mass ratio of 0.5; adding a certain amount of distilled water, stirring and mixing to prepare a 30% solution, adding a crosslinking agent epichlorohydrin according to the mass ratio of the crosslinking agent to the porous starch of 0.04%, adjusting the pH of the mixed solution to 10 by using a NaOH solution, putting the mixed solution into a water pan at 40 ℃, stirring for 12 hours, adjusting the pH of the mixed solution to 7 by using an HCl solution, washing, drying, crushing and sieving to obtain the essence wall material.
Adding distilled water into essence wall material to prepare 40% solution, adding 2% emulsifier sodium alkyl benzene sulfonate, heating and stirring in constant temperature water bath to dissolve completely, and cooling to room temperature. Slowly adding grapefruit essence (the core-wall ratio, namely the mass ratio of the essence to the essence wall material is 1.
The embedding experiment result shows that: the embedding rate of the grapefruit essence embedded by using the wall material reaches 89.32%, and after the grapefruit essence is oxidized for 12 days at 60 ℃, the peroxide value of the pure grapefruit essence is 0.7133g/100g.
Example 4
Adding water into 250g of cassava starch to prepare 40% starch milk, adjusting the pH of the solution to be =5 by using a hydrochloric acid solution, adding alpha-amylase accounting for 8% of the mass of the starch, keeping the solution at 90 ℃ for 50min, reducing the temperature to 75 ℃, continuing to convert the solution to DE to 13, rapidly heating the solution to 120 ℃ to inactivate the enzyme, and stopping the conversion. Spray drying to obtain white fine powder, and obtaining the maltodextrin.
250g of cassava starch is weighed, mixed with a sodium acetate buffer solution (pH = 6.5) to prepare 30% starch milk, stirred, mixed uniformly and preheated in a water bath at 50 ℃, and then mixed enzyme (alpha-amylase: amyloglucosidase =2. After 15h of reaction, the pH was adjusted to pH =8 with 1.5mol/L NaOH solution. Washing, drying and sieving to obtain porous starch.
Mixing maltodextrin and porous starch according to a mass ratio of 0.5; adding a certain amount of distilled water, stirring and mixing to prepare a 30% solution, adding a crosslinking agent phosphorus oxychloride according to the mass ratio of the crosslinking agent to the porous starch of 0.06%, adjusting the pH of the mixed solution to 10 by using a NaOH solution, putting the mixed solution into a water pan at 40 ℃ for stirring, adjusting the pH of the mixed solution to 7 by using an HCl solution after stirring for 12 hours, and washing, drying, crushing and sieving to obtain the essence wall material.
Adding distilled water into essence wall material to prepare 30% solution, adding 1.5% emulsifier sodium dodecyl benzene sulfonate, heating and stirring in constant temperature water bath to dissolve completely, and cooling to room temperature. Slowly adding vanilla essence (the core-wall ratio, namely the mass ratio of the essence to the essence wall material is 1.
The embedding experiment result shows that: the embedding rate of the vanilla essence embedded by using the wall material of the invention reaches 89.32%, and the peroxide value of the pure vanilla essence is 0.7133g/100g after the wall material is oxidized at 60 ℃ for 12 days.
Example 5
Adding water into 250g waxy corn starch to prepare 45% starch milk, adjusting the pH of the solution to be =6 by using hydrochloric acid solution, adding alpha-amylase accounting for 9% of the mass of the starch, keeping the solution at 85 ℃ for 60min, reducing the temperature to 70 ℃, continuing to convert the starch to DE to 14, rapidly heating the solution to 120 ℃ to inactivate the enzyme, and stopping the conversion. Spray drying to obtain white fine powder, and obtaining the maltodextrin.
250g of waxy corn starch is weighed and prepared into 30% starch milk by using sodium acetate buffer solution (pH = 5.5), stirred, mixed evenly and preheated in a water bath at 50 ℃, and mixed enzyme (alpha-amylase: amyloglucosidase = 2.5. After 8h of reaction, the pH was adjusted to pH =7 with 1mol/L NaOH solution. Washing, drying and sieving to obtain porous starch.
Mixing maltodextrin and porous starch according to a mass ratio of 0.5; adding a certain amount of distilled water, stirring and mixing to prepare a 30% solution, adding a crosslinking agent of phosphorus oxychloride and epichlorohydrin (mass ratio of 1.
Adding distilled water into the essence wall material to prepare a 40% solution, adding 2% emulsifier sodium dodecyl benzene sulfonate, heating and stirring in a constant-temperature water bath to fully dissolve the essence wall material, and cooling to room temperature. Slowly adding milk essence (the core-wall ratio, namely the mass ratio of the essence to the essence wall material is 1.
The embedding experiment result shows that: the embedding rate of the milk essence embedded by the wall material reaches 90.51 percent, and the peroxide value of the pure milk essence is 0.7133g/100g after the pure milk essence is oxidized at 60 ℃ for 12 days.
Example 6
Adding water into 300g of rice starch to prepare 35% starch milk, adjusting the pH of the solution to 6.5 by using a hydrochloric acid solution, adding alpha-amylase accounting for 10% of the mass of the starch, keeping the solution at 85 ℃ for 70min, reducing the temperature to 75 ℃, continuing to convert the solution to DE to 15, rapidly heating the solution to 120 ℃ to inactivate the enzyme, and stopping the conversion. Spray drying to obtain white fine powder, and obtaining the maltodextrin.
300g of rice starch is weighed and mixed with a sodium acetate buffer (pH = 6) to prepare 35% starch milk, the starch milk is stirred, mixed, preheated and added with a mixed enzyme (alpha-amylase: amyloglucosidase = 3. After 18h of reaction, the pH was adjusted to pH =7 with 1mol/L NaOH solution. Washing, drying and sieving to obtain porous starch.
Mixing maltodextrin and porous starch according to a mass ratio of 0.5; adding a certain amount of distilled water, stirring and mixing to prepare a 30% solution, adding a crosslinking agent sodium trimetaphosphate according to the mass ratio of the crosslinking agent to the porous starch of 0.1%, adjusting the pH of the mixed solution to 11 by using a NaOH solution, stirring in a water pan at 40 ℃, adjusting the pH of the mixed solution to 7 by using a HCl solution after stirring for 20 hours, washing, drying, crushing and sieving to obtain the essence wall material.
Adding distilled water into essence wall material to prepare 35% solution, adding 1.5% emulsifier sodium alkyl benzene sulfonate, heating and stirring in constant temperature water bath to dissolve completely, and cooling to room temperature. Slowly adding orange essence (the core-wall ratio, namely the mass ratio of the essence to the essence wall material is 1.
The embedding experiment result shows that: the embedding rate of the orange essence embedded by the wall material reaches 92.22 percent, and after the orange essence is oxidized for 12 days at 60 ℃, the peroxide value of the pure orange essence is 0.7133g/100g.
Example 7
Adding water into 300g of sweet potato starch to prepare 35% starch milk, adjusting the pH of the solution to 6.5 by using a hydrochloric acid solution, adding alpha-amylase with the mass of 6% of the starch, keeping the temperature at 85 ℃ for 80min, reducing the temperature to 75 ℃, continuing to convert the starch to DE to 16, rapidly heating to 110 ℃ to inactivate the enzyme, and stopping the conversion. Spray drying to obtain white fine powder, and obtaining the maltodextrin.
300g of sweet potato starch was weighed and mixed with a sodium acetate buffer (pH = 6.5) to prepare 45% starch milk, and after stirring, mixing and preheating in a water bath at 50 ℃, mixed enzyme (α -amylase: amyloglucosidase =2. After 21h of reaction, the pH was adjusted to pH =8 with 1.5mol/L NaOH solution. Washing, drying and sieving to obtain porous starch.
Mixing maltodextrin and porous starch according to a mass ratio of 0.5; adding a certain amount of distilled water, stirring and mixing to prepare a 30% solution, adding a crosslinking agent epichlorohydrin according to the mass ratio of the crosslinking agent to the porous starch of 0.0.3%, adjusting the pH of the mixed solution to 10 by using a NaOH solution, putting the mixed solution into a water pot at 40 ℃, stirring for 24 hours, adjusting the pH of the mixed solution to 7 by using an HCl solution, washing, drying, crushing and sieving to obtain the essence wall material.
Spray drying experimental conditions: adding distilled water into water-soluble essence wall material to prepare 35% solution, adding 1% emulsifier sodium dodecyl benzene sulfonate, heating and stirring in constant-temperature water bath to fully dissolve, and cooling to room temperature. Slowly adding bergamot essence (the core-wall ratio, namely the mass ratio of the essence to the essence wall material is 1.
The embedding experiment result shows that: the embedding rate of the wall material used for embedding the bergamot essence reaches 90.15%, and after the bergamot essence is oxidized for 12 days at 60 ℃, the peroxide value of the pure bergamot essence is 0.7133g/100g.
The present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents and are included in the scope of the present invention.

Claims (8)

1. A preparation method of a high-embedding essence microcapsule is characterized by comprising the following steps:
(1) Preparation of maltodextrin: adding water into starch to prepare 30 mass percent of starch milk, adjusting the pH value of the solution to 4.5, adding alpha-amylase accounting for 5 mass percent of the starch, keeping the solution at 85 ℃ for 20min, reducing the temperature to 60 ℃, continuing to convert the solution to a DE value of 11, inactivating the enzyme and stopping converting the solution; spray drying to obtain white fine powder to obtain maltodextrin;
(2) Preparing porous starch: preparing starch into starch milk by using a sodium acetate buffer solution, uniformly stirring and preheating in a water bath at 50 ℃, adding mixed enzyme, reacting for 6 hours, and adjusting the pH to 7; washing, drying and sieving to obtain porous starch; the mixed enzyme is formed by mixing alpha-amylase and amyloglucosidase according to the volume ratio of 1; the adding amount of the mixed enzyme is 0.5 percent of the mass of the starch; the pH value of the sodium acetate buffer solution is 5; the mass concentration of the starch milk is 30 percent;
(3) Preparing essence wall materials: mixing maltodextrin with porous starch; adding distilled water, stirring and mixing to prepare a mixed solution, adding a cross-linking agent, adjusting the pH of the mixed solution to 9, stirring at 30 ℃ for reaction for 4 hours, adjusting the pH of the mixed solution to 7, washing, drying, crushing and sieving to obtain an essence wall material; the cross-linking agent is sodium trimetaphosphate; the mass ratio of the maltodextrin to the porous starch is 0.5; the concentration of the mixed solution is 20wt%; the addition amount of the cross-linking agent is 0.01 percent of the mass of the porous starch;
(4) Preparing essence microcapsules: adding distilled water into essence wall material to prepare 20% solution, adding 0.5% emulsifier, heating and stirring in constant temperature water bath to dissolve completely, and cooling to room temperature to obtain wall material solution; adding water-soluble essence into the wall material solution, homogenizing to form uniform emulsion, and spray drying to obtain solid flowable powdered water-soluble essence microcapsule; the emulsifier is sodium dodecyl benzene sulfonate; the mass ratio of the water-soluble essence to the essence wall material is 1.
2. The method for preparing the highly-embedded essence microcapsule according to claim 1, wherein the method comprises the following steps: in the step (1), the alpha-amylase is a high-temperature-resistant enzyme.
3. The method for preparing the highly-embedded essence microcapsule according to claim 1, wherein the method comprises the following steps: in the step (1), the pH value of the solution is adjusted to 4.5 by adding hydrochloric acid.
4. The method for preparing the highly-embedded essence microcapsule according to claim 1, wherein the method comprises the following steps: in the step (1), the enzyme deactivation is realized by rapidly heating to 100 ℃.
5. The method for preparing highly-embedded essence microcapsules according to claim 1, characterized in that: in the step (2), the pH value is adjusted to 7 by adding 0.5mol/L NaOH solution.
6. The method for preparing the highly-embedded essence microcapsule according to claim 1, wherein the method comprises the following steps: in the step (3), the pH value of the mixed solution is adjusted to 7 by adding HCl solution.
7. The method for preparing highly-embedded essence microcapsules according to claim 1, characterized in that: in the step (4), the homogenization is carried out by stirring through a homogenizer; the rotating speed of the homogenizer is 12000r/min, and the homogenizing time is 30min; the water-soluble essence is lemon essence.
8. A highly-embedded essence microcapsule, which is prepared by the preparation method of any one of claims 1 to 7, and is characterized in that the embedding rate of the essence is 87.36%, and the peroxide value of the obtained water-soluble microcapsule after being oxidized for 12 days at 60 ℃ is 0.135g/100g.
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