CN112931833B - Zanthoxylum bungeanum extract microcapsule and preparation process thereof - Google Patents

Zanthoxylum bungeanum extract microcapsule and preparation process thereof Download PDF

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CN112931833B
CN112931833B CN202110294612.6A CN202110294612A CN112931833B CN 112931833 B CN112931833 B CN 112931833B CN 202110294612 A CN202110294612 A CN 202110294612A CN 112931833 B CN112931833 B CN 112931833B
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protective layer
extract
microcapsule
pricklyash peel
parts
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CN112931833A (en
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张瑞
罗璋
胡道辉
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Sichuan Xingxinsheng Biotechnology Co ltd
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Sichuan Xingxinsheng Biotechnology Co ltd
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/10Natural spices, flavouring agents or condiments; Extracts thereof
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/007Other edible oils or fats, e.g. shortenings, cooking oils characterised by ingredients other than fatty acid triglycerides
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings, cooking oils
    • A23D9/02Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
    • A23D9/04Working-up
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/03Organic compounds
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/231Pectin; Derivatives thereof
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/256Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from seaweeds, e.g. alginates, agar or carrageenan
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/269Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of microbial origin, e.g. xanthan or dextran
    • A23L29/272Gellan
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/275Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of animal origin, e.g. chitin
    • A23L29/281Proteins, e.g. gelatin or collagen
    • A23L29/284Gelatin; Collagen
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/30Foods 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
    • A23L29/35Degradation products of starch, e.g. hydrolysates, dextrins; Enzymatically modified starches
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00Shaping or working of foodstuffs characterised by the products
    • A23P10/30Encapsulation of particles, e.g. foodstuff additives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00Shaping or working of foodstuffs characterised by the products
    • A23P10/30Encapsulation of particles, e.g. foodstuff additives
    • A23P10/35Encapsulation of particles, e.g. foodstuff additives with oils, lipids, monoglycerides or diglycerides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02Making microcapsules or microballoons
    • B01J13/04Making microcapsules or microballoons by physical processes, e.g. drying, spraying
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02Making microcapsules or microballoons
    • B01J13/04Making microcapsules or microballoons by physical processes, e.g. drying, spraying
    • B01J13/046Making microcapsules or microballoons by physical processes, e.g. drying, spraying combined with gelification or coagulation
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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Abstract

The invention discloses a pricklyash peel extract microcapsule which comprises 10-20 parts of pricklyash peel extract, 50-200 parts of a first protective layer, 150-600 parts of a second protective layer and 2-20 parts of a third protective layer, wherein the pricklyash peel extract is sequentially wrapped by the first, second and third protective layers. Wherein the fructus Zanthoxyli extract is selected from any one of fructus Zanthoxyli essential oil or fructus Zanthoxyli oleoresin. The microcapsule of the pricklyash peel extract prepared by the invention has stronger stability, and can protect the tingling and fragrance of the pricklyash peel extract under the damage of oxygen, pH value, moisture, temperature and the like. The microcapsule of the pricklyash peel extract prepared by the invention is used in the composite seasoning, can effectively keep the flavor of pricklyash peel, and can resist 100 ℃ for more than 30 minutes in the cooking process, and delay the release of aroma and spicy substances.

Description

Zanthoxylum bungeanum extract microcapsule and preparation process thereof
Technical Field
The invention belongs to the field of biology, and particularly relates to the technical field of embedding. Relates to a pricklyash peel extract microcapsule and a preparation process thereof, and the pricklyash peel extract microcapsule prepared by the preparation process.
Background
At present, the research on chemical components of the pepper extract mainly aims at three components of volatile oil, amides and alkaloids, wherein the two flavor components of the volatile oil and the amides respectively reflect the aroma and the tingling characteristics of the pepper, and the pepper is used in the food industry and mainly takes the aroma and the tingling of the pepper, so that the three components are the two most important characteristic indexes in the quality evaluation of the pepper. In addition, other physiologically active components such as lignans, coumarin, fatty acids, flavonoid glycosides and triterpenes are contained in Zanthoxylum bungeanum. Sterols, and the like.
The xanthoxylin, namely the xanthoxylin oleoresin, is mainly chain unsaturated amide, contains a large amount of conjugated triene bonds, is extremely easy to oxidize, the xanthoxylin extract is slowly oxidized in the storage process because of containing the xanthoxylin substances, mainly lipid is directly reacted with oxygen, namely automatic oxidation, most of the reaction is free radical chain reaction, peroxide, hydroperoxide and peroxy acid are usually generated, and the peroxide value is increased because of the formation of various peroxides. The intermediate products are unstable and continue to react to finally generate aldehydes, ketones, alcohols, hydrocarbons and the like with rancidity characteristics, in addition, light, enzymes and metal ions can catalyze the oxidation process in the automatic oxidation process to accelerate the oxidation, and if the peroxide value increases rapidly in the shelf life, the flavor loss is large. The aroma components of the pricklyash peel essential oil have partial volatile components, and the volatile components are lost with the increase of the ambient temperature in the storage and use processes, so that the incomplete and missing of the aroma are easily caused.
The microencapsulation of the pricklyash peel extract can effectively protect the chemical components of the pricklyash peel, provide stability, reduce the damage of external environment (such as oxygen, pH value, moisture, temperature and the like), and particularly has oxidation damage effect; controlling or extending the release rate of the core material; isolating components that diversify the food system without interfering with each other is a difficulty that must be overcome in the current industry. The prior invention CN109907125A discloses a zanthoxylum oil resin microcapsule with improved stability and a preparation method thereof, wherein the zanthoxylum oil resin microcapsule is subjected to high-speed homogenizing and stirring to form O/W emulsion, and spray drying is carried out to obtain zanthoxylum oil resin microcapsule powder. Meanwhile, the microcapsule wall material is very easy to dissolve in water, so that the zanthoxylum oil resin is quickly dissolved in the water in the boiling process, and the release speed of the zanthoxylum oil resin is high, so that the release is not facilitated.
Based on the above, the zanthoxylum bungeanum extract microcapsule which is applied to the composite seasoning has strong stability, can resist high temperature in the cooking process, and can slowly release the fragrant substances and the spicy substances, and the preparation process thereof are urgently needed in the industry.
Disclosure of Invention
In view of the above analysis, the present invention aims to provide a microcapsule of pricklyash peel extract, which further improves the stability of pricklyash peel extract, is used in composite flavoring, maintains the flavor of pricklyash peel, and can resist high temperature and delay release during cooking. The invention is realized by the following processes:
a zanthoxylum bungeanum extract microcapsule comprising:
fructus Zanthoxyli extract;
a first protective layer;
a second protective layer; and
a third protective layer;
the pricklyash peel extract is sequentially wrapped by a first protective layer, a second protective layer and a third protective layer;
the grain diameter of the microcapsule is 0.5-5 mm.
Further, the pepper extract is 10-20 parts, the first protective layer is 50-200 parts, the second protective layer is 150-600 parts, and the third protective layer is 2-20 parts.
Further, the pricklyash peel extract is selected from pricklyash peel essential oil or pricklyash peel oleoresin;
wherein the fructus Zanthoxyli essential oil is fructus Zanthoxyli essential oil 180, lot number 20200903 provided by Chongqinghua extract biotechnology limited company.
The zanthoxylum oleoresin is zanthoxylum oleoresin LH2202 provided by Longide and extraction technology Co., ltd., batch No. 20210114.
Further, the first protective layer is selected from porous dextrin or modified starch as a medium, preferably porous dextrin.
Further, the second protective layer is selected from palm oil or shortening as a medium, preferably palm oil.
Further, the third protective layer is formed by a cross-linking reaction between a hydrogel medium and calcium ions; the hydrogel medium is selected from any one of sodium alginate, pectin, gellan gum and gelatin.
A process for preparing a zanthoxylum bungeanum extract microcapsule, comprising:
(1) Preparation of the Zanthoxylum bungeanum extract coated with the first protective layer:
dispersing the first protective layer in water to form supersaturated solution, keeping constant stirring at normal temperature, after dissolving the pepper extract with equal amount of ethanol, dripping the solution into the supersaturated solution at constant speed and continuously stirring for about 4 hours, standing overnight, fully adsorbing the pepper extract, filtering, and washing with clear water for 3 times to obtain the pepper extract wrapped by the first protective layer, wherein the pepper extract is 10-20 parts by weight, and the first protective layer is 50-200 parts by weight;
(2) Preparation of a second protective layer:
melting the second protective layer into liquid at 60 ℃, uniformly dispersing the pricklyash peel extract wrapped by the first protective layer, which is obtained in the step (1), continuously stirring, and keeping the temperature constant at 60 ℃ to obtain a second protective layer product, wherein the second protective layer product is 150-600 parts by weight;
(3) Preparation of a third protective layer:
preparing the third protective layer into an aqueous solution with the weight of 1-2%, wherein a cold water bath is an aqueous solution of calcium lactate with the weight of 5%, using concentric shaft tube equipment, enabling an inner layer with the diameter of 0.3-3 mm to flow into a second protective layer product, enabling an outer layer with the diameter of 1-5 mm to flow into the third protective layer product, enabling the third protective layer product to flow out simultaneously, wrapping the second protective layer by the third protective layer, dripping the second protective layer product into the cold water bath, and enabling the third protective layer product to be quickly solidified, wherein the third protective layer product is 2-20 parts by weight;
(4) And (3) forming:
and (3) carrying out normal-temperature ventilation drying on the third protective layer product obtained in the step (3) to obtain the zanthoxylum bungeanum extract microcapsule.
The invention also discloses a pepper extract microcapsule prepared by any one of the preparation processes.
The invention also discloses application of any one of the pepper extract microcapsules in food flavoring technology.
The invention has the beneficial effects that:
1. the microcapsule of the pricklyash peel extract prepared by the invention has stronger stability, and can protect the tingling and fragrance of the pricklyash peel extract under the damage of oxygen, pH value, moisture, temperature and the like.
2. The microcapsule of the pricklyash peel extract prepared by the invention is used in a composite seasoning, can effectively keep the flavor of pricklyash peel, and can resist 100 ℃ for more than 30 minutes in the cooking process, and delay the release of aroma and spicy substances.
Drawings
FIG. 1 is a schematic diagram of the structure of the Zanthoxylum bungeanum extract microcapsule of the present invention.
Fig. 2 is a schematic structural view of the concentric shaft tube of the present invention.
Detailed Description
Example 1
A process for preparing a zanthoxylum bungeanum extract microcapsule, comprising:
(1) Preparation of the Zanthoxylum bungeanum extract coated with the first protective layer:
dispersing porous dextrin as a medium in water to form supersaturated solution, keeping constant stirring at normal temperature, uniformly dripping the equal amount of ethanol into the supersaturated solution after dissolving the pepper essential oil, continuously stirring for about 4 hours, standing overnight, fully adsorbing the pepper extract, filtering, and washing with clear water for 3 times to obtain the pepper extract wrapped by the first protective layer, wherein the pepper essential oil is 15 parts by weight, and the first protective layer is 125 parts by weight;
(2) Preparation of a second protective layer:
melting palm oil as a medium at 60 ℃ to form liquid, uniformly dispersing the pricklyash peel extract wrapped by the first protective layer obtained in the step (1), continuously stirring, and keeping the temperature constant at 60 ℃ to obtain a second protective layer product, wherein the second protective layer is 375 parts by weight;
(3) Preparation of a third protective layer:
preparing an aqueous solution with the weight of 1.5% by taking sodium alginate as a medium, preparing an aqueous solution with the weight of 5% of calcium lactate in a cold water bath, enabling an inner layer with the diameter of 2mm to flow a second protective layer product and an outer layer with the diameter of 3mm to flow a third protective layer product by using concentric shaft tube equipment, enabling the third protective layer product to flow out simultaneously, wrapping the second protective layer product, dripping the second protective layer product into the cold water bath, and rapidly solidifying the third protective layer product to form a third protective layer product, wherein the third protective layer product is 10 parts by weight;
(4) And (3) forming:
and (3) carrying out normal-temperature ventilation drying on the third protective layer product obtained in the step (3), thus obtaining the capsicum annuum extract microcapsule with the particle size of 3mm.
Example 2
A process for preparing a zanthoxylum bungeanum extract microcapsule, comprising:
(1) Preparation of the Zanthoxylum bungeanum extract coated with the first protective layer:
dispersing modified starch as a medium in water to form supersaturated solution, keeping constant stirring at normal temperature, after dissolving pepper oleoresin with equal amount of ethanol, dripping into the supersaturated solution at constant speed and continuously stirring for about 4 hours, standing overnight, fully adsorbing the pepper extract, filtering, and washing with clear water for 3 times to obtain the pepper extract wrapped by the first protective layer, wherein the pepper extract is 10 parts by weight, and the first protective layer is 50 parts by weight;
(2) Preparation of a second protective layer:
melting shortening serving as a medium into liquid at 60 ℃, uniformly dispersing the pepper extract wrapped by the first protective layer, which is obtained in the step (1), in the liquid, continuously stirring, and keeping the temperature constant at 60 ℃, so as to obtain a second protective layer product, wherein the second protective layer product is 150 parts by weight;
(3) Preparation of a third protective layer:
preparing a water solution with the weight of 1% by taking gellan gum as a medium, preparing a calcium lactate water solution with the weight of 5% by taking a cold water bath, enabling an inner layer with the diameter of 0.3mm to flow a second protective layer product by using concentric shaft tube equipment, enabling an outer layer with the diameter of 1mm to flow a third protective layer product, enabling the third protective layer product to flow out simultaneously, wrapping the second protective layer by the third protective layer, dripping the second protective layer product into the cold water bath, and enabling the third protective layer product to be quickly solidified, wherein the third protective layer product is 2 parts by weight;
(4) And (3) forming:
and (3) carrying out normal-temperature ventilation drying on the third protective layer product obtained in the step (3), thus obtaining the capsicum annuum extract microcapsule with the particle size of 4mm.
Example 3
A process for preparing a zanthoxylum bungeanum extract microcapsule, comprising:
(1) Preparation of the Zanthoxylum bungeanum extract coated with the first protective layer:
dispersing porous dextrin serving as a medium in water to form supersaturated solution, keeping constant stirring at normal temperature, dissolving the pepper essential oil with equal amount of ethanol, dripping the solution into the supersaturated solution at constant speed, continuously stirring for about 4 hours, standing overnight, fully adsorbing the pepper extract, filtering, and washing with clear water for 3 times to obtain the pepper extract wrapped by the first protective layer, wherein the pepper extract is 20 parts by weight, and the first protective layer is 200 parts by weight;
(2) Preparation of a second protective layer:
melting shortening serving as a medium into liquid at 60 ℃, uniformly dispersing the pepper extract wrapped by the first protective layer, which is obtained in the step (1), in the liquid, continuously stirring, and keeping the temperature constant at 60 ℃, so as to obtain a second protective layer product, wherein the second protective layer is 600 parts by weight;
(3) Preparation of a third protective layer:
preparing pectin as a medium into 2% by weight of aqueous solution, preparing a cold water bath into 5% by weight of calcium lactate aqueous solution, enabling an inner layer with the diameter of 3mm to flow into a second protective layer product by using concentric shaft tube equipment, enabling an outer layer with the diameter of 5mm to flow into a third protective layer, enabling the third protective layer to flow out simultaneously, wrapping the second protective layer, dripping the second protective layer into the cold water bath, and rapidly solidifying the third protective layer to form a third protective layer product, wherein the third protective layer is 20 parts by weight;
(4) And (3) forming:
and (3) carrying out normal-temperature ventilation drying on the third protective layer product obtained in the step (3), thus obtaining the capsicum annuum extract microcapsule with the particle size of 5mm.
Comparative example 1
Reference is made to the technical process disclosed in application number CN201910083905.2, which is specifically as follows:
(1) The ultraviolet lamp tube with the power of 20W in the ultra-clean bench is turned on and preheated for 20min, so that the light wave is stabilized at 253.7nm. The zein powder was spread on a glass petri dish 9cm in diameter and then placed under a vertical ultraviolet lamp at a distance of 20cm for irradiation for 30min.
(2) 15.0g of the above-treated zein powder was weighed, 250mL of distilled water was added thereto, and the mixture was stirred with a magnetic stirrer for 1 hour to prepare a suspension of 6.0% (w/v). After 30min treatment at 500w ultrasonic power, 4000r/min centrifugation is carried out for 10min to remove insoluble substances, and 2.0% (w/v) of corn protein powder solution is prepared.
(3) Uniformly mixing the corn gluten meal solution and chitosan oligosaccharide according to the mass ratio of 1:2, dissolving and dispersing the mixture in 250mL of distilled water, and stirring the mixture for 12 hours by a magnetic stirrer to uniformly mix the mixture. The pH of the mixed solution was adjusted to 8.0 and heated in a water bath at 80℃for 2h.
(3) And then regulating the pH value of the reactant to 3.0 after the corn protein and chitosan oligosaccharide aqueous bath heating reaction, then adding 250mL of Arabic gum solution, enabling the mass ratio of the chitosan oligosaccharide to the Arabic gum in the mixed solution to be 2:8, enabling the solid concentration to be 0.96% (w/v), and cooling to room temperature after continuously heating in a water bath at 80 ℃ for 10 hours.
(4) And then adding 0.2g of grape wine peel residue polysaccharide (the mass percentage accounts for 4.0% of the total wall material) into the reaction liquid, and stirring and mixing uniformly until the total wall material concentration in the mixture reaches 1.0% (w/v). Taking the mixture as a wall material, adding 5.0g of pepper oleoresin, keeping the mass ratio of the core wall at 1:1, and emulsifying at 30 ℃ for 10min at 10000r/min to form O/W emulsion.
(5) And (3) spray-drying the O/W type emulsion under the conditions that the air inlet temperature is 180 ℃, the air outlet temperature is 80 ℃ and the sample injection speed is 9mL/min to obtain the zanthoxylum oil resin microcapsule powder.
The embedding rate of the microcapsule of the zanthoxylum oil resin prepared under the condition of the embodiment is 64.5%, and the content of the zanthoxylum oil is 6.5%; the peroxide value of the grease at 65 ℃ is 16.9mmol/kg in 21 days of the accelerated oxidation experiment, and the peroxide value of the non-embedded zanthoxylum oleoresin is 42.6mmol/kg.
Comparative example 2
The purchased fructus Zanthoxyli essential oil is 180, and the lot number is 20200903 provided by Chongqinghua extract biotechnology limited company.
Comparative example 3
The purchased zanthoxylum oleoresin is zanthoxylum oleoresin LH2202 and batch No. 20210114 provided by the company of Shangnan Liand extraction technology.
Test example 1
Detection of tingling substances of each group of samples at different time points
Taking samples of each group of examples and comparative examples of unit mass respectively, extracting the spicy substances of the samples, preparing standard substances with different concentrations by taking hydroxy-alpha-sanshool as a standard substance, drawing a standard curve, detecting by using a high performance liquid chromatography, and determining the hydroxy-alpha-sanshool content of each group of examples and comparative examples of unit mass.
The samples of each group of examples and comparative examples were measured and sampled at each time node when they were put into clear water having ph=7 and heated at 100 ℃ for 60 minutes, and the change in the content of dissolved hydroxy- α -sanshool in each group of samples in water was detected based on the hydroxy- α -sanshool content data of each group of examples and comparative examples per unit mass obtained in the above steps, and further the change in the tingling ingredients was detected, as shown in table 1.
TABLE 1 detection of the tingling substances of the groups at different time points
Figure DEST_PATH_IMAGE002
The data according to table 1 shows: the samples of example 1, example 2 and example 3 were heated at 100 ℃, the spherical microcapsules were not completely broken yet, and slow release at high temperature could be achieved; although the slow release can be realized in comparative example 1, the slow release system is completely destroyed at 15-30 minutes, and the hydroxyl-alpha-sanshool continuously decays along with high temperature; comparative examples 2 and 3 showed continuous decay of hydroxy-alpha-sanshool at high temperature without the protection of a slow release system.
Test example 2
The environmental impact of each set of samples of examples and comparative examples was determined: comprises oxidizing each group of samples, and reacting for 60min in an acidic environment and a neutral environment. The performance of each set of samples was tested and the specific results are shown in table 2.
Taking samples of each group of examples and comparative examples of unit mass respectively, extracting the spicy substances of the samples, preparing standard substances with different concentrations by taking hydroxy-alpha-sanshool as a standard substance, drawing a standard curve, detecting by using a high performance liquid chromatography, and determining the hydroxy-alpha-sanshool content of each group of examples and comparative examples of unit mass.
The samples of each group of examples and comparative examples were measured and sampled at each time node when they were put into clear water at ph=5 and ph=7 and heated at 100 ℃ for 60 minutes, and the change in the content of dissolved hydroxy- α -sanshool in each group of samples in water was detected based on the hydroxy- α -sanshool content data of each group of examples and comparative examples obtained by the above steps, and further the change in the tingling ingredients was detected, as shown in table 2.
TABLE 2 detection of the tingling substances of the groups at different time points under different pH environments
Figure DEST_PATH_IMAGE004
The data according to table 2 shows: the slow release effect of the example 1 and the example 2 under the acidic condition is better than that of the neutral environment, and the microcapsule presents certain acid resistance; example 3, in acidic and neutral environments, the slow release effect of the microcapsules is not very different; comparative example 2 and comparative example 3 are not strong in the acid and neutral environment sensitivity of the environment, and the appearance of the dissolution appearance of the hydroxy-alpha-zanthoxylum is not changed obviously; in comparative example 1, the emulsion system was destroyed under acidic conditions, and the microcapsule had poor slow release performance and was not resistant to acidic environments.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.

Claims (7)

1. A zanthoxylum bungeanum extract microcapsule comprising:
10-20 parts of pricklyash peel extract;
50-200 parts of a first protective layer;
150-600 parts of a second protective layer; and
2-20 parts of a third protective layer;
the pricklyash peel extract is sequentially wrapped by a first protective layer, a second protective layer and a third protective layer;
the grain diameter of the microcapsule is 0.5-5 mm;
wherein the first protective layer is selected from porous dextrin or modified starch as a medium;
the second protective layer is selected from palm oil or shortening oil as a medium;
the third protective layer is formed by the cross-linking reaction of the hydrogel medium and calcium ions.
2. The microcapsule according to claim 1, wherein:
the fructus Zanthoxyli extract is selected from fructus Zanthoxyli essential oil or fructus Zanthoxyli oleoresin.
3. The microcapsule of claim 1, wherein: the hydrogel medium is selected from any one of sodium alginate, pectin, gellan gum and gelatin.
4. A process for preparing the pepper extract microcapsule of any one of claims 1-3, comprising:
(1) Preparation of the Zanthoxylum bungeanum extract coated with the first protective layer:
dispersing the first protective layer in water to form supersaturated solution, keeping constant stirring at normal temperature, dissolving the pricklyash peel extract with equal amount of ethanol, dripping into the supersaturated solution at constant speed for full adsorption, filtering and washing to obtain the pricklyash peel extract wrapped by the first protective layer;
(2) Preparation of a second protective layer:
melting the second protective layer into liquid at 60 ℃, and uniformly dispersing the pricklyash peel extract wrapped by the first protective layer obtained in the step (1) into the liquid to obtain a second protective layer product;
(3) Preparation of a third protective layer:
the concentric shaft tube device is utilized, the inner layer flows into the second protective layer, the outer layer flows into the third protective layer, the inner layer and the outer layer flow out simultaneously, and the third protective layer is rapidly solidified to form a third protective layer product;
(4) And (3) forming:
and (3) carrying out normal-temperature ventilation drying on the third protective layer product obtained in the step (3) to obtain the zanthoxylum bungeanum extract microcapsule.
5. The manufacturing process of claim 4, wherein:
the concentric shaft tube comprises an inner tube and an outer tube, the diameter of the inner tube is 0.3-3 mm, and the diameter of the outer tube is 1-5 mm.
6. A microcapsule of zanthoxylum bungeanum extract prepared according to any one of the preparation processes of claims 4 or 5.
7. Use of a pepper extract microcapsule according to any one of claims 1-3, or 6 in a food perfuming technology.
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