Fish oil microcapsules production method

FIELD: food industry.

SUBSTANCE: organoleptical properties improvement is achieved by the fish oil microcapsules production method characterised by obtainment of an oil-in-water emulsion by way of mixing fish oil and an encapsulation ingredient in water; the components are taken at a ratio 30-35 and 25-30 wt %, water - balance; the method additionally involves homogenisation and dispersion of the obtained emulsion in an ultrasonic field and microemulsion subsequent spray drying; ultrasonic dispersion is carried out with insonification frequency equal to 28 kHz and intensity equal to 40 W/cm2; spray drying is carried out with a parallel hot air flow with the temperature at the inlet and outlet equal to 160-180°C respectively.

EFFECT: simplification and enhancement of microencapsulation processes efficiency during production of deodorised and encapsulated fat-soluble food products, in particular, improvement of organoleptic properties of fish oils used for food products enrichment.

4 cl, 6 ex, 1 tbl

 

The invention relates to food production, namely the production of deodorized and encapsulated fat-soluble foods, in particular fish oils, as well as to the production of microcapsules preventive food additives used for the enrichment of food products in different food industries, such as dairy, bakery, food concentrates, and others.

To remove volatile components, which can cause problems with smell and color in the final product based on fish fat, makes fat an odor, use a number of ways deodorization of fish fats. For example,

- fish oils deodorization with steam under vacuum at 230°C (Pat. USA N4874629, CL. A23D 5/00, publ. 1989). The method allows to remove volatile components that give Giroud a specific smell, but it leads to a certain reduction in the proportion of fatty acids such as omega-3, isomerization and polymerization of the latter, which reduces its quality,

- deodorization with the use of vapors of acetic acid for carrying out the process in more mild conditions (Pat. Of the Russian Federation No. 2039795, SW 3/14, A23L 1/325, publ. 20.07.1995)

- deodorization of fat in the deodorizer at a temperature of 220-230°C and a residual pressure of 0.13 to 0.4 kPa. In the reaction zone deodorizer injected organic sulfonation (Pat. Of the Russian Federation No. 2242508, SW 3/14, publ. 20.12.2004) �whether using one or more adsorption columns, containing adsorbent material to remove impurities (Pat of the Russian Federation No. 2515970, SW 3/06, publ.20.05.2014),

- deodorization of oils and fats, which would provide a deaeration, heating, distillation and cooling, before the distillation of oil and grease last treated in a constant magnetic field with magnetic induction of 0.8-1.2 TL at a linear velocity of flow in the 1.5-2.0 m/s (Pat. Of the Russian Federation No. .2100427, SW 3/00, publ. 27.12.1997 G.).

However, increasing the treatment temperature leads to a slight decrease in the proportion of fatty acids such as omega 3, isomerization and polymerization of the latter due to high temperature, which reduces its quality and does not lead to dispersion of fat. Moreover, according to these methods it is impossible to obtain a fine fat.

One of the promising directions deodorization of fish oil in dietary supplements for maximum masking of taste and smell, as well as enhancing solubility and uniformity of distribution when administered in food products without altering their traditional appearance, consistency and taste is encapsulation. Encapsulation is a process to enable particles of a substance in a thin shell of film-forming material. The most common encapsulation used for obtaining microcapsules of drugs.

So, in us Pat. RF 209255 (IPC A61K 047/02, publ. 10.10.1997) proposed a method of obtaining a solid pharmaceutical preparation comprising preparing a mixture of active ingredient with the excipient, mixing by abrasion.

As the filler used submicroscopic pyrogenic silica, and a mixture of active ingredient and submicroscopic pyrogenic silica prepared in a ratio providing a coating of particles of the active ingredient submicroscopic pyrogenic silica, and stirring the mixture lead by crushing and abrasion until, while uncoated particles of the active ingredient will not disappear from the field of view of the microscope, for 1.5-3.5 h. the resulting product can be described as nanocapsule, in the future, after the process of coating the active ingredient silica particles can be administered orally.

The disadvantages of this method are the duration of the process and the need to implement every half hour of monitoring the state of the particles in the cooking process under the electron microscope.

In us Pat. Of the Russian Federation No. 2095055 (A61K 9/52, publ. 10.11.1997) a method of producing a solid non-porous microspheres, which comprises melting pharmaceutically inactive substance carrier, the dispersion of the pharmaceutically active substance in the melt in an inert atmosphere, the spray�received their dispersion in the form of a mist in the freezing chamber under pressure, in an inert atmosphere, at a temperature from -15°C to -50°C and separation of the obtained microspheres into fractions by size.

Disadvantages of the proposed method are the complexity and duration of the process. The need for special equipment.

In us Pat. Of the Russian Federation No. 2359662 (A61K 009/56, publ. 27.06.2009) a method of producing microcapsules using spray cooling dispersant components in the spray tower Niro under the following conditions: air temperature at the inlet 10°C, the temperature at the outlet 28°C, the speed of rotation of the spray drum 10000 rpm/min Microcapsules according to the invention have improved stability and provide adjustable and/or prolonged release of the active ingredient.

The disadvantages of the proposed method are the duration of the process.

In us Pat. WO/2011/127030 US, (A61K 8/11; B01J 2/00; publ. 13.10.2011) proposed several methods for producing microcapsules: interfacial polymerization, thermoinduced phase separation, spray drying, evaporation of the solvent, etc.

The disadvantages of the proposed methods is the complexity, the duration of the processes.

The method, taken as a prototype, is a method of producing microcapsules described in the patent application of the Russian Federation No. 2006108860, B01J 13/04 publ. 27.09.2007.

The method comprises the steps:

- obtaining the aqueous phase with rastvorennye active ingredients

- obtaining a hydrophobic phase in molten form, which is used as animal oils, fatty acids, monoglycerides, etc.,

- dissolution in any of the phases of the encapsulated substance selected from the group comprising gel forming colloids such as sodium alginate, hydrocolloids, starch, pectin, gelatin, cititzen or any mixture forming a gel colloids,

- homogenization or mixing the combined phases of the emulsion water-in-oil and

- subsequent encapsulation of the resulting emulsion by means of gelation, crosslinking, fusion or agglomeration.

In the process of using the heating phase, the pressure variation at the individual stages, the stage of microcapsular lead by cooling in a fluidized bed and spray cooling.

The thus obtained microcapsules comprise from about 1 to 100 water droplets included in the hydrophobic shell matrix.

The disadvantage of this method is the complexity and duration of the process, the necessity for special equipment, and the low yield of the desired capsules.

Furthermore, the method does not allow to completely remove volatile components, to ensure the maximum masking of the taste and smell of the fish are fat and don't allows get use a capsule for introduction into food products.�you because the latter do not have sufficient solubility and uniformity of their distribution when administered in food.

The object of the invention is to simplify and improve the process of microencapsulation.

The technical result of the invention is the lack of technological losses in the production of the product and improvement of its organoleptic characteristics.

The problem is solved by a method of production of fish oil microcapsules, characterized by the emulsion oil-in-water by mixing in water fish oil and encapsulating the component, in the ratio of 30-35 and 25-30 wt.%, the rest - water, homogenizing dispersing the resulting emulsion in an ultrasonic field and subsequent spray drying of the microemulsion, ultrasonic dispersion with a frequency of scoring 28 kHz and an intensity of 40 W/cm2and spray drying are parallel stream of hot air with a temperature at the inlet and outlet respectively of 160-180°C and not more than 50°C.

Mainly as encapsulating agent used modified starch.

Usually ultrasonic dispersion are not more than 10 minutes, and spray drying does not exceed 10.

The method is as follows.

The method was aprobaron raw materials - fish grease "Hey�onol" (TU 9197-004-29388404-08).

Eikonal mixed with modified starch, the resulting mixture is dispersed in water, homogenized with obtaining microemulsions and subjected to the spray-drying of microemulsion with obtaining fine powder. The ratio of components in the mixture by dispersing the following (in wt.%): fish oil "Eikonal" - 30-35, modified starch - 25-30, the rest is water.

Homogenization is carried out by means of an ultrasonic homogenizer with a frequency of scoring 28 kHz with an intensity of 40 W/cm2for 10 min in a volume of emulsion 1. In the process of spray drying microemulsion spray in the parallel stream of hot air in a special chamber with the temperature of the air inlet 180°C, and 50°C. moreover, due to the large surface area of atomized emulsion, a high temperature gradient at the initial stage of the process and turbulente airflow, the drying speed is high enough. The residence time of the product in the chamber does not exceed 10 s. in addition, the emulsion is not exposed to high temperature as it is cooled by absorbing heat by evaporation of water from the emulsion composition. The powder together with air leaves the drying chamber and is trapped by a cyclone, then it will be removed from the cyclone and Packed.

The conditions of the process of microencapsulation by locatio�inflammatory drying predetermines stringent requirements for functional properties of the materials used.

To ensure high content of fish oil "Eikonal" in encapsulating a mixture of 40-60% and thereby reduce losses during drying, and to improve the performance of your equipment kapsuliruemogo substance must have a high solubility in water.

For a homogeneous and durable shell on the surface of drops of fish oil "Eikonal" it is necessary for encapsulating a substance has high stabilizing ability, good film-forming properties and also retains plasticity throughout the range of drying temperatures. Encapsulating component was selected modified starch, as well as in the process of microencapsulation, the content of fish oil "Eikonal" must not exceed the emulsifying capacity of the encapsulating material, the starch was taken in the claimed ratio.

The efficiency of the process of microencapsulation depends on the fineness of the emulsion (average particle size). Size reduction of fat particles in an innovative way ultrasonic dispersion with frequency scoring 28 kHz and an intensity of 40 W/cm2to 1-4 microns and a narrow size distribution contributes to the stabilization of emulsions and increases the efficiency of drying.

Upon completion of the spray drying process have evaluated the effectiveness of microencapsulation and deodorization. Definition�their total number decapsulating fish oil "Eikonal" in dry form was performed by high performance capillary gas chromatography after extraction of fish oil "Eikonal" of dry product. Capsulesbuy capacity of the drug was evaluated on the content decapsulating fish oil "Eikonal" in 100 grams of the drug. The efficiency of the process of microencapsulation was calculated as the ratio of the number decapsulating fish oil "Eikonal" to the original content in the system (%). Estimation in 100 grams of dry product was introduced 60 grams of fish oil "Eikonal", which corresponded to almost 100%, i.e. without process losses when the residual moisture content of 2-4%. The efficiency of the process of microencapsulation by spray drying amounted to 80-90%, it was noted the complete absence of the smell of fish oil "Eikonal" that undoubtedly positively differentiates this method of deodorizing from analogs and prototypes.

Example 1

350 g fish fat Eikonal (TU 9197-004-29388404-08), 250 g of modified starch (Hi-Cap 100, Germany, cGy EN.77.99.21.009 E. 014581.10.12) and 400 g of water (SanPiN 2.1.4.1074) mix in the jars with a capacity of 2 liters.

The receptacle containing the mixture was placed in an ultrasonic homogenizer series of Alain and dispersed at 28 kHz, 40 W/cm210 min.

After dispersing the resulting microemulsion is sent to the spray dryer and spray when the inlet temperature of 180°C and outlet - 50°C.

Received 550 g of microcapsules ranging in size from 2 to 4 microns.

The diameter of the microcapsules, micron and their share in %

2,0 - 70, 3,0 - 20, 4,0 - 10, 5,0 - no

ODS�neigh Eikonal capsules 34%, capsules odorless fish, comments on the quality of capsules - no.

Examples No. 2-6 are given in the table.

The results of the research (examples 1-6) have been meet samples (examples 1, 3, 4) the requirements of regulations.

Thus, the invention provides a deodorizing fish oil "Eikonal" and allows to expand the range of products enriched Akinola" as a source of essential polyunsaturated fatty acids ω-3.

Obtaining a particulate microencapsulated powder fish oil "Eikonal" gives a widely known food fish fat "Eikonal" new consumer quality, allows you to open new possibilities of application and the effects of drugs, prevention of its damage under the influence of the environment, and it provides prolonged absorption from the gastrointestinal tract.

1. A method of producing microcapsules fish oil, characterized by the emulsion oil-in-water by mixing in water fish oil and encapsulating the component, in the ratio of 30-35 and 25-30 wt.%, the rest - water, homogenizing, dispersing the resulting emulsion in an ultrasonic field and subsequent spray drying of the microemulsion, ultrasonic dispersion with a frequency of scoring 28 kHz and an intensity of 40 W/cm2and R�spiritello drying are parallel stream of hot air with a temperature at the inlet and outlet respectively of 160-180°C and not more than 50°C.

2. A method according to claim 1, characterized in that the encapsulating agent is used modified starch.

3. A method according to claim 1, characterized in that the ultrasonic dispersing lead not more than 10 minutes.

4. A method according to claim 1, characterized in that the spray drying are not more than 10 seconds.



 

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