CN110522061B - Microcapsule and preparation method thereof - Google Patents

Microcapsule and preparation method thereof Download PDF

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CN110522061B
CN110522061B CN201910800038.XA CN201910800038A CN110522061B CN 110522061 B CN110522061 B CN 110522061B CN 201910800038 A CN201910800038 A CN 201910800038A CN 110522061 B CN110522061 B CN 110522061B
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oil
alginate
microcapsule
wall material
acid
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CN110522061A (en
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赵澎
苏娟
王文静
赵美法
吕海金
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Qingdao Spata Analysis Testing Co ltd
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Qingdao Technical College
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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
    • A23L29/015—Inorganic compounds
    • 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
    • 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
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/115—Fatty acids or derivatives thereof; Fats or oils
    • 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
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/115—Fatty acids or derivatives thereof; Fats or oils
    • A23L33/12—Fatty acids or derivatives thereof
    • 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
    • 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
    • A23P10/35—Encapsulation of particles, e.g. foodstuff additives with oils, lipids, monoglycerides or diglycerides
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Chemical & Material Sciences (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nutrition Science (AREA)
  • Molecular Biology (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Mycology (AREA)
  • Inorganic Chemistry (AREA)
  • Biophysics (AREA)
  • Medicinal Preparation (AREA)
  • Manufacturing Of Micro-Capsules (AREA)
  • General Preparation And Processing Of Foods (AREA)

Abstract

The invention relates to the technical field of oil-containing microcapsules, and discloses a microcapsule and a preparation method thereof. The preparation method comprises the steps of embedding the oil by adopting a wall material-water-soluble alginate in a Venturi embedding mode, carrying out surface layer solidification on the obtained oil micro-droplets wrapped by the alginate by adopting a calcium salt, and finally embedding and agglomerating two pairs of solidified microcapsules by adopting the wall material to obtain the microcapsule powdered oil. The invention directly forms alginate into microcapsule wall embedding grease and obtains dry microcapsule powder, and the oil carrying capacity and the capsule wall stability of the obtained microcapsule are greatly improved.

Description

Microcapsule and preparation method thereof
Technical Field
The invention relates to the technical field of oil-containing microcapsules, in particular to a microcapsule and a preparation method thereof.
Background
In the food industry, liquid oil cannot be conveniently and directly added into solid food, the microcapsule technology wraps oil tiny liquid drops through specific wall material to enable the oil tiny liquid drops to be in a solid powder state, the application of the oil in the aspects of food and nutrition additives is expanded, and meanwhile, the wall material of the microcapsule can protect the oil in the microcapsule from being oxidized by external oxygen and sensitive substances to a certain degree.
The construction of microcapsule wall and the screening of wall material affect the oxidation resistance and stability of the final finished microcapsule, which is also a major technical problem encountered in the application of microcapsule technology in the food industry. At present, the preparation method of the microcapsule mainly utilizes wall materials such as vegetable gum, starch materials or protein to primarily wrap oil droplets, and the wrapping is generally realized by utilizing the processes of shearing, stirring, homogenizing and the like of the oil in a water-soluble system; starch and protein are mixed to be used as wall materials to reduce cost and improve application performance, in the prior art, the sodium alginate addition amount is small, the sodium alginate mainly plays a role of an emulsifier, so that the compound emulsion wraps oil droplets, but the interaction between wall material molecules in the compound emulsion is weak, the formed microcapsule wall cannot be effectively and tightly attached to liquid, looseness or holes can be generated, and the microcapsule wall is easily exposed to high-temperature airflow in the spray drying process to cause oxidation risk, in the prior art, the wall material embedding is generally carried out in a multi-shearing and homogenizing mode to enhance the oxidation stability of microcapsules so as to solve the problems, but the wall materials are easily repeatedly accumulated on the oil droplets in the shearing and stirring embedding mode, so that the microcapsule wall has less oil content and reduced oil carrying capacity, and therefore, under the existing microcapsule structure and process, oil loading and stability are a contradictory problem.
The above-mentioned prior art has already been disclosed, for example, chinese patent application CN201810864212.2 discloses that sodium alginate is used to construct microcapsule wall to prepare water-soluble component microcapsule, this patent first uses the emulsion containing sodium alginate to embed water-soluble anthocyanin, then uses calcium alginate to solidify the capsule wall to obtain wet microcapsule in the form of micro-droplet, for example, chinese patent application CN201611069040.7 discloses that the above-mentioned method is used to embed water-soluble fucoxanthin, both of the above-mentioned two patent applications are used to embed water-soluble component, and belong to the existing technology of embedding oil in water (water-soluble component) first, and then embedding oil, this patent discloses the method can not embed oil, and the product is wet microcapsule droplet, and does not have the basic technical characteristics of powder microcapsule. For example, chinese patent applications CN201610339011.1 and CN201410792977.1 disclose respectively preparing perilla oil and DHA microcapsules using sodium alginate as a wall material component, and the above-mentioned technology also belongs to the existing conventional industrial microcapsule preparation method, and has the problem of reduced oil carrying capacity due to multiple embedding, the oil carrying capacity can only reach 30% at most, and the stability is also poor.
In view of the above problems, the present invention provides a new method for preparing microcapsules, wherein alginate directly forms microcapsule wall embedding grease and obtains dry microcapsule powder by utilizing venturi effect, so as to enhance the stability of microcapsule wall and increase the oil carrying capacity of microcapsule powder, and thus the microcapsule powder is more suitable for being widely applied in food industry.
Disclosure of Invention
The invention provides a microcapsule and a preparation method thereof, aiming at solving the technical problems of low oil-carrying capacity and poor stability of the microcapsule in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention aims to provide a preparation method of microcapsules, which is characterized in that wall material-water-soluble alginate is adopted to embed grease in a Venturi embedding mode, the surface layer of grease micro-droplets wrapped by the obtained alginate is solidified by calcium salt, and finally, wall material-two pairs of solidified microcapsules are adopted to embed and agglomerate to obtain microcapsule powdered grease.
According to the invention, by utilizing the characteristics of an alginate solution and utilizing a Venturi embedding mode, the alginate forms a spherical microcapsule outer wall with a monolayer structure, and is compact and complete under the action of surface tension, the flow velocity of a Venturi tube is high, the sodium alginate cannot be repeatedly stacked on the grease, and the thickness of the formed wet microcapsule wall is extremely small through instantaneous calcification, so that the volume of a micro-droplet can be controlled within the range of 5nm-0.5cm, and a large amount of grease is wrapped in the monolayer capsule wall, thereby solving the problem of low oil loading of the microcapsule in the prior art; the alginate forms the spherical microcapsule outer wall with compact and complete structure on the surface of the atomized oil micro-droplet due to the action of surface tension, the combination capacity of the capsule outer wall material and the oil is strong, the oxidation stability of the microcapsule is enhanced, and the microcapsule is particularly suitable for embedding the easily oxidized polyunsaturated fatty acid oil, so that the invention improves the oxidation stability of the microcapsule while ensuring the oil carrying capacity.
The obtained alginate-coated oil micro-droplets are calcified to obtain high-compactness calcium alginate gel, the calcified microcapsule wall is insoluble in water, the capsule wall has thermal irreversibility, the stability in subsequent thermal treatment is higher than that of microcapsule powder prepared by a shearing emulsifying embedding technology, and the problem of oxidation of embedded oil in the processing process can be effectively solved. The wet microcapsule is difficult to dry due to the characteristic of calcium alginate gel, so the invention adopts the wall material to embed and agglomerate the solidified microcapsule, and has better application adaptability compared with the wet microcapsule wrapped by pure calcium alginate gel.
Preferably, the preparation method of the microcapsule specifically comprises the following steps:
S1the oil is decompressed and atomized by a Venturi tube to form micro liquid drops, and a wall material, namely water-soluble alginate aqueous solution enters through a suction inlet of the Venturi tube and is adsorbed on the surfaces of the micro liquid drops to form oil micro liquid drops wrapped by alginate; the mass concentration of the alginate solution is 0.5-5%, and the mass ratio of the grease to the alginate solution is 1: 10-50;
S2directly spraying the alginate-coated oil micro-droplets into a calcium salt aqueous solution from the venturi tube, and carrying out surface layer solidification on the alginate micro-droplets coated with the oil by using the calcium salt to obtain oil-in-water microcapsules; the mass fraction of the calcium salt in the calcium salt water solution is 0.1-5%;
S3and carrying out secondary embedding and agglomeration on the microcapsules by adopting a wall material pair to obtain microcapsule powdered oil, wherein the wall material I accounts for 60-100% of the total wall material.
The existing microcapsule processing technology generally uses a shearing emulsification technology, microcapsule emulsion needs to be homogenized, the microcapsule emulsion cannot be cleaned after homogenization, spray drying must be directly carried out, redundant alginate is brought in the drying process, so that the microcapsules are adhered and agglomerated, and qualified products cannot be obtained2And then the oil-in-water microcapsule obtained is subjected to low-speed centrifugation to remove most of water, and can be washed for multiple times in the centrifugation step to remove redundant alginate in the solution, and the rotation speed of the low-speed centrifugation is 1500 rpm. The calcified microcapsules are centrifuged to realize the function of cleaning the microcapsules, redundant alginate is washed away, and fluidized bed precipitation is carried outWhen the microcapsule is embedded with the powder, no bonding balls are generated between the microcapsule glue.
Preferably, the calcium salt is selected from CaCl2、CaSO4、Ca(NO3)2、Ca2(PO4)3Calcium lactate, calcium gluconate or calcium citrate.
The oil or fat is not particularly limited as long as it is an oil or fat that can be used in the food industry, and preferably, the oil or fat provided by the present invention may be one or more of microbial oil, animal oil or fat, and vegetable oil or fat.
Preferably, the microbial oil contains 5% by mass or more of fatty acid; the fatty acid is one or more of docosapentaenoic acid (DPA), docosahexaenoic acid (DHA), arachidonic acid (ARA), eicosapentaenoic acid (EPA) or tetracosenoic acid; the microbial oil can be directly purchased from the market, and can also be prepared by a method of microbial strain fermentation.
Preferably, the vegetable oil is essential oil or contains more than 5% of one or more of Conjugated Linoleic Acid (CLA), alpha-linolenic acid, gamma-linolenic acid or tetracosenoic acid by mass percent. The vegetable oil can be directly purchased from the market, and can also be prepared by pressing or extracting; the essential oil is selected from one or more of lemon essential oil, mint essential oil, jojoba essential oil, lavender essential oil, tea tree essential oil, frankincense essential oil, orange peel essential oil, wormwood essential oil, silybum marianum seed essential oil, sea buckthorn fruit oil, sea buckthorn seed oil, lemon grass essential oil or bergamot essential oil.
Preferably, the animal oil is one or more of antarctic krill oil, fish oil, seal oil and seal oil, and the fish oil contains more than 5% of DHA and EPA in mass percentage.
Furthermore, the oil can also comprise corresponding fatty acid methyl ester, ethyl ester and glyceride prepared by using the animal, plant and microbial oil as a raw material in a transesterification mode and the like, and also comprises high-purity fatty acid and esters thereof prepared by using the obtained fatty acid methyl ester or ethyl ester as a raw material.
The wall material-water-soluble alginate provided by the invention is selected from one or more of sodium alginate, potassium alginate, ammonium alginate, propylene glycol alginate, triethanolammonium alginate and dibutylamine alginate.
The second wall material provided by the invention is one or more selected from modified starch, cyclodextrin, maltodextrin, pregelatinized starch or octenyl succinic acid esterified starch.
Another object of the present invention is to provide a microcapsule, wherein the volume average particle size of the microcapsule powder is in the range of 50nm to 1cm, the microcapsule comprises a core material and a wall material, the core material accounts for 50 to 80% of the mass of the microcapsule, the wall material comprises a first wall material and a second wall material, and the first wall material accounts for 60 to 100% of the mass of the wall material; the core material is one or more of microbial oil, animal oil or vegetable oil, the wall material I is one or more of sodium alginate, potassium alginate, ammonium alginate, propylene glycol alginate, triethanolammonium alginate or dibutylamine alginate, and the wall material II is one or more of modified starch, cyclodextrin, maltodextrin, pregelatinized starch or octenyl succinate starch.
The invention finishes the embedding of the grease by using the embedding mode of the Venturi tube, the grease pumped from the liquid inlet is decompressed and atomized to form micro-droplets when passing through the Venturi tube, the alginate entering from the suction inlet is adsorbed on the surface of the grease micro-droplets due to the Venturi effect, and the alginate forms the spherical microcapsule outer wall with a compact and complete structure on the surface of the atomized grease micro-droplets due to the action of surface tension. Meanwhile, the wet microcapsule wall formed by the method provided by the invention has extremely small thickness, and a large amount of grease can be wrapped in the wet microcapsule wall, so that the problem of low oil-carrying capacity of the microcapsule in the prior art is solved. The microcapsule powder obtained by the technical scheme in the embedding mode of the Venturi tube has the volume average particle size of 50nm-1cm, the maximum oil carrying rate can reach 85%, and the embedding rate is higher than 99%.
Drawings
Fig. 1 is a process flow diagram of a microcapsule preparation method provided by the present invention.
Detailed Description
The invention discloses a microcapsule and a preparation method thereof, and the microcapsule can be realized by appropriately improving process parameters by referring to the content in the text by the technical personnel in the field. It is expressly intended that all such similar substitutes and modifications which would be obvious to those skilled in the art are deemed to be included in the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The following detailed description of the invention refers to specific embodiments thereof for better understanding by those skilled in the art.
Example 1
Dissolving 25g sodium alginate in 5L water, dissolving DHA microbial oil (Qingdao Youlan biotechnology, Inc.) 500g, and mixing water jet type Venturi tube (SSQ-125, 3mm nozzle caliber, 0.7 m)3Flow/h) is connected with a micro magnetic pump (MP10R, Shanghai Kurui pump valve manufacturing Co., Ltd.) through a pressure-resistant vacuum tube, DHA grease is pumped into the inlet of the Venturi tube, sodium alginate solution is sucked from the suction port of the Venturi tube (see figure 1), and atomized wet microcapsules enter 10L 1% of CaCl2And (2) carrying out capsule wall solidification in the solution for 1min, centrifuging and washing the solidified wet microcapsule particles at low speed of 1500 revolutions, introducing the particles into a fluidized bed (WBF1G, Van military drying equipment Co., Ltd., Changzhou city), preparing dry microcapsule powder by using modified starch as an embedding agent, spraying 200g of the modified starch by adopting a top spraying mode, introducing air at 60 ℃, drying the particles by using hot air at 80 ℃ after embedding to obtain a product, and recycling the redundant starch by the fluidized bed.
Example 2
Dissolving 250g potassium alginate in 5L water, dissolving 100g oleum Lini (inner Mongolia red well oil Co., Ltd.) in water, mixing water jet type Venturi tube (SSQ-125, 3mm nozzle caliber, 0.7 m)3Flow/h) was connected to a micro magnetic pump (MP10R, manufactured by Shanghai Kurui pump valve Co., Ltd.) via a pressure-resistant vacuum tube, linseed oil was pumped into the inlet of the venturi tube, potassium alginate solution was sucked from the suction port of the venturi tube, and atomized wet microcapsules were introduced into 10L of 0.1% CaSO4And (2) carrying out capsule wall solidification in the solution for 2min, centrifuging and washing the solidified wet microcapsule particles at low speed of 1500 revolutions, entering a fluidized bed (WBF1G, Van army drying equipment Co., Ltd., Changzhou city), preparing dry microcapsule powder by using the octenyl succinate starch as an embedding agent, spraying 180g of the octenyl succinate starch by adopting a top spraying mode, carrying out air inlet temperature of 70 ℃, drying by using hot air at 80 ℃ after embedding to obtain a product, and recycling the redundant starch by the fluidized bed.
Example 3
Dissolving 100g ammonium alginate in 5L water, preparing tuna oil (Taicang Norshinou Biotechnology Co., Ltd.) 166g, and mixing with water jet type Venturi tube (SSQ-125, 3mm nozzle diameter, 0.7 m)3Flow/h) and a micro magnetic pump (MP10R, manufactured by Shanghai Kurui pump valve Co., Ltd.) through a pressure-resistant vacuum tube, tuna oil is pumped into the inlet of the Venturi tube, sodium alginate solution is sucked from the suction port of the Venturi tube (figure 1), and the atomized wet microcapsules are filled with 20L 2% Ca (NO)3)2And (2) carrying out capsule wall solidification in the solution for 2min, centrifuging and washing the solidified wet microcapsule particles at low speed of 1500 revolutions, introducing the particles into a fluidized bed (WBF1G, Van army drying equipment Co., Ltd., Changzhou city), preparing dry microcapsule powder by using the octenyl succinate esterified starch as an embedding agent, spraying 600g of the octenyl succinate esterified starch by a top spraying mode, introducing air at 70 ℃, drying the embedded product by using hot air at 80 ℃ to obtain a product, and shaking and falling the redundant starch by the fluidized bed for recycling.
Example 4
Dissolving 50g of triethanolammonium alginate in 5L of water, preparing jojoba essential oil (green source essential oil refinery of Jian city) 200g, and spraying water type Venturi tube (SSQ-125, 3mm nozzle)Bore diameter of 0.7m3Flow rate) is connected with a micro magnetic pump (MP10R, Shanghai Kurui pump valve manufacturing company, Ltd.) through a pressure-resistant vacuum tube, jojoba oil is pumped into the inlet of a Venturi tube, sodium alginate solution is sucked from the suction port of the Venturi tube (figure 1), atomized wet microcapsules are put into 5L 5% calcium lactate solution for capsule wall solidification, the solidification time is 1min, solidified wet microcapsule particles are centrifuged and washed at low speed of 1500 rpm and enter a fluidized bed (WBF1G, Van army drying equipment company, Ltd., Changzhou city), octylsuccinate starch is used as embedding agent to prepare dry microcapsule powder, 200g of octylsuccinate starch is sprayed in a top spraying mode, the air inlet temperature is 50 ℃, the product is obtained by drying with hot air at 60 ℃ after embedding, and redundant starch is recycled by the fluidized bed.
Example 5
Dissolving 200g propylene glycol alginate in 5L water, preparing jojoba essential oil (green source essential oil refinery of Jian city) 200g, and mixing with water jet type Venturi tube (SSQ-125, 3mm nozzle diameter, 0.7 m)3Flow rate) is connected with a micro magnetic pump (MP10R, Shanghai Kurui pump valve manufacturing company, Ltd.) through a pressure-resistant vacuum tube, jojoba oil is pumped into the inlet of a Venturi tube, sodium alginate solution is sucked from the suction port of the Venturi tube (figure 1), atomized wet microcapsules enter 5L 1.5% calcium gluconate solution for capsule wall solidification, the solidification time is 1min, solidified wet microcapsule particles are washed by 1500 rpm low-speed centrifugal water and enter a fluidized bed (WBF1G, Van Jun drying equipment company, Ltd.), dry microcapsule powder is prepared by using pregelatinized starch as an embedding agent, 200g of pregelatinized starch is sprayed in a top spraying mode, the inlet air temperature is 50 ℃, the product is obtained by drying with 60 ℃ hot air after embedding, and redundant starch is recycled by the fluidized bed.
Example 6
Dissolving 300g sodium alginate in 30L water, preparing OPO structure fatty oil (lodes-Crocoka corporation) 600g, and mixing water jet type Venturi tube (SSQ-150, 4mm nozzle caliber, 1.18 m)3Flow/h) and a micro magnetic pump (MP20R, Shanghai Kurui pump valve manufacturing Co., Ltd.) through a pressure-resistant vacuum tube, pumping OPO structure fat and oil into the inlet of the Venturi tube, and sodium alginateThe solution is sucked from a suction port of a Venturi tube (figure 1), atomized wet microcapsules are put into 100L of 3 percent calcium citrate solution for capsule wall solidification, the solidification time is 2min, solidified wet microcapsule particles are subjected to low-speed centrifugation at 1500 rpm, water washing and then enter a fluidized bed (WBF2G, Van Jun drying equipment Co., Ltd., Changzhou city), octyl succinate starch is used as an embedding agent to prepare dry microcapsule powder, 2000g of maltodextrin is sprayed in a top spraying mode, the air inlet temperature is 70 ℃, hot air drying at 80 ℃ is used for obtaining a product after embedding, and redundant maltodextrin is recycled by the fluidized bed.
Example 7
Dissolving 25g sodium alginate in 5L water, dissolving DHA microbial oil (Qingdao Youlan biotechnology, Inc.) 500g, and mixing water jet type Venturi tube (SSQ-125, 3mm nozzle caliber, 0.7 m)3Flow/h) is connected with a micro magnetic pump (MP10R, Shanghai Kurui pump valve manufacturing Co., Ltd.) through a pressure-resistant vacuum tube, DHA grease is pumped into the inlet of the Venturi tube, sodium alginate solution is sucked from the suction port of the Venturi tube (figure 1), atomized wet microcapsules are put into 10L 1% CaCl2And (2) carrying out capsule wall solidification in the solution for 5min, centrifuging and washing the solidified wet microcapsule particles at low speed of 1500 revolutions, introducing the particles into a fluidized bed (WBF1G, Van military drying equipment Co., Ltd., Changzhou city), preparing dry microcapsule powder by using cyclodextrin as an embedding agent, spraying 150g of cyclodextrin in a top spraying manner at the air inlet temperature of 80 ℃, drying the particles by using hot air at the temperature of 100 ℃ after embedding to obtain a product, and recycling the redundant cyclodextrin by the fluidized bed.
Example 8
The microcapsules prepared in examples 2, 5 and 7 and the commercially available microcapsules were subjected to an oxidation acceleration test by an oven method to measure the stability of each microcapsule, 5g of the sample was placed in an oven at 80 ℃ for 24 hours of forced air oxidation, and the oil extraction was performed to measure the peroxide number, the embedding rate, the surface oil and the moisture, and the measurement results are shown in table 1, wherein 1 day of the accelerated oxidation corresponds to 24 days in a normal state.
TABLE 1 results of property measurement of microcapsules obtained in examples 2, 5 and 7
Figure BDA0002182067060000071
The data in table 1 show that the microcapsules prepared in examples 2, 5 and 7 have excellent embedding rate and the oil loading reaches more than 50%; after 24h accelerated test, the peroxide value is still lower than 5.0meq/Kg, accords with relevant national standards, has better oxidation stability compared with the commercially available microcapsule product, and simultaneously the surface oil index of the microcapsule product is also lower than the commercially available product. Therefore, the oil loading capacity and the oxidation stability of the microcapsule obtained by the preparation method provided by the invention are greatly improved, and the technical problems of low oil loading capacity and poor oxidation stability of the microcapsule in the prior art are solved.
Comparative example 1
Dissolving 5g sodium alginate solution in 500g water, stirring, heating in water bath, adding emulsifier glycerol fatty acid ester, mixing to obtain wall material solution, adding core material DHA microbial oil 50g (Qingdao Youlan biological science and technology Co., Ltd.), stirring at 2000 rpm for 3min to obtain sodium alginate-embedded DHA oil emulsion, and dripping 1L10g/L CaCl with concentration of 1L10g/L into the emulsion with 10ml syringe2Calcifying for 3min in the solution, and filtering to obtain microcapsule oil drop embedded by sodium alginate. The method is similar to the technical scheme disclosed in the patent application CN 201611069040.7.
Comparative example 2
25g of whey protein, 1g of sodium alginate, 1g of monoglyceride as an emulsifier and 1g of antioxidant D-sodium erythorbate palmitate, putting the materials into 500mL of hot water of 75 ℃, stirring, keeping the temperature and dissolving for 30min, and cooling to 50 ℃ to obtain an aqueous phase liquid; adding 12.5 g of DHA microbial oil (Qingdao Youlan biological science and technology limited) into the uniformly mixed oil-soluble antioxidant vitamin E, and continuously stirring to obtain a core material for later use after the mixture is uniform; adding the core material into the aqueous phase liquid, continuously stirring, firstly shearing at low speed for 20min at 500 revolutions, then shearing for 3min at 5000 revolutions to obtain emulsion, then homogenizing the emulsion twice, wherein the first homogenizing pressure is 25MPa, the second homogenizing pressure is 20MPa, then carrying out sterilization treatment, carrying out spray drying on the sterilized emulsion, leading the air inlet temperature to be 80 ℃, and then passing through a 60-mesh vibrating screen to finally obtain 100g of DHA microbial oil powder. The method is similar to the technical scheme disclosed in the patent application CN 201410792977.1.
The microcapsules obtained in example 7 and comparative examples 1 and 2 were tested for their performance and the results are shown in table 2.
Table 2 comparison of properties of microcapsules obtained in example 7 and comparative examples 1 and 2
Figure BDA0002182067060000081
The data in table 2 show that the microcapsule prepared in comparative example 1 is a wet-surface micro-droplet, does not have the technical characteristics of the dry microcapsule powder prepared in the present application, and cannot be applied to solid powder food, and the microcapsule prepared in example 7 disclosed in the present invention is a solid powder microcapsule, has low water content and high economical efficiency, can be applied to various forms of food such as solid liquid, and the like, and has significant improvement in practicability. Secondly, the diameter of the particles of the wet microcapsule prepared in the comparative example 1 is 10 to 30 times larger than that of the wet microcapsule prepared in the example 7, the wet microcapsule is used as a liquid drop and is not resistant to mechanical pressure, the calcium alginate wall is broken after grinding and extrusion, and the embedded grease is easy to leak out, and the technical problem is solved by the scheme of the embodiment 7 of the invention. The comparative example 2 adopts sodium alginate as an emulsifier component, the sodium alginate accounts for less than 1% of the wall material, starch and protein are used as the wall material, microcapsule liquid drops are formed through modes of multiple shearing homogenization and the like, and then microcapsule powdered oil is obtained through spray drying, the traditional process belongs to the traditional process, the oil carrying amount is 12%, the oil carrying amount is far lower than 85% of that of the example 7 of the invention, the energy consumption of the homogeneous shearing and drying is about 30 yuan RMB/kg, the energy consumption cost estimated in the example 7 is about 10 yuan RMB/kg due to the fact that the spray drying process with high energy consumption is avoided, and the market application value is huge.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (9)

1. A preparation method of microcapsules is characterized in that wall material-water-soluble alginate is adopted to embed grease in a Venturi embedding mode, obtained alginate-coated grease micro-droplets are subjected to surface layer solidification by calcium salt, and finally wall material-two pairs of solidified microcapsules are adopted to embed and agglomerate to obtain microcapsule powder grease; the preparation method comprises the following steps:
S1the oil is decompressed and atomized by a Venturi tube to form micro liquid drops, and a wall material, namely water-soluble alginate aqueous solution enters through a suction inlet of the Venturi tube and is adsorbed on the surfaces of the micro liquid drops to form oil micro liquid drops wrapped by alginate; the mass concentration of the alginate solution is 0.5-5%, and the mass ratio of the grease to the alginate solution is 1: 10-50;
S2directly spraying the alginate-coated oil micro-droplets into a calcium salt aqueous solution from the Venturi tube, and carrying out surface layer solidification on the alginate micro-droplets coated with the oil by using the calcium salt to obtain oil-in-water microcapsules; the mass fraction of the calcium salt in the calcium salt water solution is 0.1-5%;
S3carrying out secondary embedding and agglomeration on the microcapsules by adopting a wall material to obtain microcapsule powdered oil; the first wall material accounts for 60-100% of the total mass of the wall material.
2. The method of claim 1, wherein step S2Centrifuging and washing the obtained oil-in-water microcapsule; the rotational speed of the centrifuge was 1500 rpm.
3. The method of claim 1, wherein the calcium salt is selected from the group consisting of CaCl2、CaSO4、Ca(NO3)2、Ca2(PO4)3Calcium lactate, calcium gluconate or calcium citrate.
4. The method for preparing microcapsules of claim 1, wherein the oil is one or more of microbial oil, animal oil or vegetable oil.
5. The method according to claim 4, wherein the microbial oil is a mixture containing 5% by mass or more of a fatty acid; the fatty acid is one or more of docosapentaenoic acid (DPA), docosahexaenoic acid (DHA), arachidonic acid (ARA), eicosapentaenoic acid (EPA) or tetracosenoic acid.
6. The method according to claim 4, wherein the vegetable oil or fat is an essential oil or contains at least 5% by mass of one or more of Conjugated Linoleic Acid (CLA), alpha-linolenic acid, gamma-linolenic acid, and tetracosenoic acid; the animal oil is one or more of antarctic krill oil, fish oil, seal oil and seal oil, and the fish oil contains more than 5% of DHA and EPA in mass percentage.
7. The method according to claim 1, wherein the water-soluble alginate is selected from one or more of sodium alginate, potassium alginate, ammonium alginate, propylene glycol alginate, triethanolammonium alginate and dibutylamine alginate.
8. The preparation method of claim 1, wherein the wall material II is one or more selected from modified starch, cyclodextrin, maltodextrin, pregelatinized starch and octenyl succinate starch.
9. The microcapsule prepared by the preparation method according to any one of claims 1 to 8, wherein the average particle size of the microcapsule body is in the range of 50nm to 1cm, the microcapsule comprises a core material and a wall material, the core material accounts for 50 to 80 percent of the mass of the microcapsule, the wall material comprises a first wall material and a second wall material, and the first wall material accounts for 60 to 100 percent of the mass of the wall material; the core material is one or more of microbial oil, animal oil or vegetable oil, the wall material I is one or more of sodium alginate, potassium alginate, ammonium alginate, propylene glycol alginate, triethanolammonium alginate or dibutylamine alginate, and the wall material II is one or more of modified starch, cyclodextrin, maltodextrin, pregelatinized starch or octenyl succinate starch.
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CN111468050A (en) * 2020-04-29 2020-07-31 福州大学 Method for preparing composite essential oil particles based on microfluidic technology
CN111617052B (en) * 2020-05-30 2022-04-08 广东紫薇星健康产业有限公司 Seal oil microcapsule and preparation method thereof
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS58205463A (en) * 1982-05-24 1983-11-30 Q P Corp Granules for fruit juice, its production and beverage containing the same
US5744337A (en) * 1995-12-26 1998-04-28 The United States Of America As Represented By The Secretary Of The Navy Internal gelation method for forming multilayer microspheres and product thereof
CN103458709A (en) * 2011-01-21 2013-12-18 凡赛尔医药股份有限公司 Microencapsulated probiotic substance and process of manufacture
CN103610010A (en) * 2013-11-14 2014-03-05 扬州大学 Fabrication method of pepper oleoresin microcapsule
CN104334032A (en) * 2012-05-24 2015-02-04 弗门尼舍有限公司 Hybrid coacervate capsules
CN105852131A (en) * 2016-04-11 2016-08-17 华中农业大学 Method for preparing organic food processing standard meeting fish oil microcapsules

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS58205463A (en) * 1982-05-24 1983-11-30 Q P Corp Granules for fruit juice, its production and beverage containing the same
US5744337A (en) * 1995-12-26 1998-04-28 The United States Of America As Represented By The Secretary Of The Navy Internal gelation method for forming multilayer microspheres and product thereof
CN103458709A (en) * 2011-01-21 2013-12-18 凡赛尔医药股份有限公司 Microencapsulated probiotic substance and process of manufacture
CN104334032A (en) * 2012-05-24 2015-02-04 弗门尼舍有限公司 Hybrid coacervate capsules
CN103610010A (en) * 2013-11-14 2014-03-05 扬州大学 Fabrication method of pepper oleoresin microcapsule
CN105852131A (en) * 2016-04-11 2016-08-17 华中农业大学 Method for preparing organic food processing standard meeting fish oil microcapsules

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