RU2291701C2 - Method for production of ultradispersed powder from unossified antlers of maral and siberian stag - Google Patents

Abstract

FIELD: biotechnology, food processing industry, medicine.

SUBSTANCE: claimed method includes unossified antler cutting, freezing and crushing together with skin or wool and skin to produce particles having size of at most 0.5 mm, drying and additional crushing in jet mill to produce particles having size of at most 0.1-30.0 mum. Drying of crushed frozen material is carried out simultaneously with additional crushing in jet mill, in gas medium flow with humidity of at most 10 mass % wherein temperature of gas flow in jet mil is automatically maintained at +50°C or less. Produced target ultradispersed powder contains non-radioactive carbon isotope C¹³ in amount of at least 1.3 % based on total carbon content in finished product. Frozen and crushed material is periodically loaded into jet mill with interval sufficient to produce yield of 70 mass % or more. Period of simultaneous drying and crushing of one material portion between loading cycles is not longer than 1.5-5 hours.

EFFECT: simplified technology, target bioactive product of improved quality.

3 cl, 3 ex, 1 tbl, 2 dwg

Description

The invention relates to a technology for processing, preserving and storing raw materials of natural origin, in particular antlers of deer and sika or reindeer, to obtain biologically active crushed dry material, which can be used to obtain preparations in the form of powders and liquid extracts in the medical industry for immunostimulating means in biotechnology to obtain stimulators of the growth of microorganisms in the biochemical industry as a feedstock for oia hormones and biologically active peptides in the food industry as flavoring, mineral and vitamin supplements.

Antlers during cutting contain about 70-80% of water. Their processing and preservation pursue the following objectives: storage for a long time; preservation of biologically active substances in them; creation of conditions for the most complete extraction of their existing principles from antlers.

A known method of drying a thermolabile material used in the pharmaceutical and food industries, including grinding this material, placing it in a chamber, evacuating to a pressure of 10 ^-1 mbar and drying the material to a residual moisture content of not more than 5 wt.% (Germany patent No. 2914181, IPC F 26 B 5/04, publ. 1982).

However, when using this method for processing and preserving freshly cut antlers, it has the following disadvantages. Freshly cut antlers have high humidity (water content up to 70-80%), as a result of which, when grinding, the product particles stick together in large conglomerates and the drying process is significantly lengthened, and after drying additional grinding of dry material is required.

A known method of continuous drying of food and drugs, including drying the product in a fluidized bed with air, having a temperature of + 90-130 ° C and a speed of 0.8-2.0 m / s, to a dry matter content of 75-90 wt.%. Semi-dry product is placed in a vacuum chamber and dried at a temperature of 25-45 ° C and a pressure of 1-10 mm Hg. to a dry matter content of 98 wt.% (international application No. PCT (WO) 81/01415, IPC C 12 N 1/18, publ. 1981).

However, this method is unacceptable for preserving antlers, because the final product in dry form loses a number of thermolabile biologically active substances under the action of high temperature. A known method of drying food under vacuum, including freezing the product, placing it in the chamber and creating a reduced pressure in it. During the drying process in the chamber, the medium temperature is gradually raised to 30-45 ° C and the product is dried at this temperature to a residual moisture content of 3.0-5.0 wt.% (US patent N 4520574, IPC F 26 V 5/06, publ. 1985).

However, the technological process of drying the material is long (3-5 days) and energy intensive due to the low rate of moisture removal from the material.

A known method of preserving antlers, including heat treatment of antlers with their subsequent cooling. Moreover, the heat treatment is carried out in a steam atmosphere at a temperature increase from +35 to 85 ° C for 1-1.5 minutes, and subsequent cooling is carried out at room temperature (+ 15-20 ° C) for 2-3 minutes. Heat treatment and cooling are carried out repeatedly (USSR copyright certificate N 528915, IPC ⁶ A 01 N 1/02, publ. 1976).

However, the method provides insufficient preservation of biologically active substances contained in antlers during their preservation.

A known method of preserving antlers, including preliminary exposure of antlers at a temperature of (+4) - (- 20) ° C for 7-30 days. Then they are heat-treated with dry heat at a temperature of + 70-72 ° C for 4 hours at atmospheric pressure. After time, the temperature in the heat chamber is reduced to + 40 ° C, the antlers are moved to a wind dryer, where they dry for 24-72 hours. The alternation of heat treatment with drying in the wind is carried out 4-5 times (copyright certificate No. 1106466, IPC ⁶ A 01 N 1/02, publ. 07.08.84).

However, the process of preserving antlers has a long duration (more than 35 days), in which part of the thermolabile biologically active substances is lost under the influence of high temperature.

There is a method of drying reindeer antlers with air, comprising the first stage of heating the antlers to 35 ° C and keeping them at this temperature for 1 hour, then in the second stage the heating temperature of the antlers is increased to 70 ° C and again kept for 1 hour, and in the third stage heating temperature is reduced to 45 ° C and also maintained at this temperature for 1 hour. After the period of heating the antlers is completed, they are cooled by air to room temperature for 6 hours. The treatment cycle is repeated many times until the antlers of the desired moisture content are obtained. The drying process lasts 3-5 days (USSR author's certificate No. 1205860, IPC ⁶ A 01 N 1/00, F 26 B 3/02, publ. 23.01.86).

However, this process of preserving antlers also has a long duration (more than 5 days), in which part of the thermolabile biologically active substances is lost under the influence of high temperature.

There is a known method of processing reindeer antlers, including drying the antlers in three stages, while in the first stage the antlers are heated to + 68-70 ° C, dried for 4 hours at an air temperature of + 70-72 ° C and ventilation drying is carried out for 48 hours, repeating the cycle from 1 to 3 times. In the second stage, the antlers are heated to + 65 ° C, drying with hot air is carried out at + 65-68 ° C for 4 hours, ventilation drying is carried out for 48-72 hours. In the third stage, drying is carried out in a draft for 4-10 days, depending on the size of the antlers (RF patent No. 2034553, IPC ⁶ A 61 K 35/32, publ. 05/10/95).

However, this process of preserving antlers also has a long duration (more than 25 days), in which part of the thermolabile biologically active substances is lost under the influence of high temperature.

A known method of preparing deer antlers for pantocrine, including washing the antlers, immersing the antlers for 0.5-2.0 minutes in liquid nitrogen, removing hair from frozen skin mechanically, sawing the antlers into separate pieces, followed by grinding the antlers in any known manner (patent RF №2082407, IPC ⁶ A 61 K 35/00, publ. 06/27/97).

The disadvantage of this method is that in the process of short-term exposure to antlers of liquid nitrogen, they do not have time to freeze over the entire cross section, as a result of which when grinding antlers with high humidity (water content up to 70-80%), the product particles stick together in large conglomerates and, in the case of preparation of powders requires a longer drying time, increased energy consumption and additional grinding of the dry preparation.

A known method of processing and preserving antlers for the subsequent isolation of biologically active substances from it, including cleaning raw antlers from the skin, freezing the cleaned antlers at a temperature of minus 3-10 ° C, grinding the antlers into pieces 0.5-1 cm in size and freeze-drying the material according to the standard method. Lyophilized dried crushed antlers are ground to a powder state (RF patent No. 2054292, IPC ⁶ A 61 K 35/32, publ. 02.20.96).

However, this method of processing and preserving antlers also has several disadvantages. When cleaning raw antlers from the skin, a part of the biologically active substances contained in the skin is lost. The insufficient degree of antler freezing, when crushed, leads to the adhesion of particles and the formation of large conglomerates, which lengthens the drying process of the material. The standard freeze drying technique has high energy consumption and insufficient moisture removal, which increases the drying time.

A known method of preserving antlers, including cutting and preliminary cleaning of the antlers from the skin, freezing them at a temperature of -40 ° C and storage, if necessary, at this temperature. Antlers are dried at a temperature of from -40 ° C to + 45 ° C and a pressure of 0.5 mm Hg. to a residual moisture content of 10-11%. The drying process lasts more than 24 hours (copyright certificate No. 563146, IPC ⁶ A 01 N 1/02, publ. 06/30/77).

However, this method of processing and preserving antlers has several disadvantages. When cleaning raw antlers from the skin, a part of the biologically active substances contained in the skin is lost. The technology does not provide for preliminary grinding of antlers, which significantly lengthens the drying time. In addition, the drying process provides insufficient moisture removal, which also increases the drying time.

The closest analogue (prototype) is a method of processing and preserving antlers of deer and sika deer, including cutting antlers, freezing and storing this raw material in a frozen state and drying it in a chamber under vacuum. Moreover, the antlers are frozen and stored in a thermostat in liquid nitrogen; before drying, the frozen antlers are crushed together with the skin or with the skin and skin to particles no larger than 500 microns in size. Drying in a chamber of frozen crushed material under vacuum is carried out in the pressure range of 0.1-10.0 mm Hg at temperatures from -60 ° C to + 30 ° C to a residual moisture content of not more than 5 wt.%, and after drying, the material is additionally crushed to a particle size of 0.1-30.0 μm. Processing antlers with the skin or with the hair and skin can reduce the loss of biologically active substances. Grinding antlers before drying can reduce drying time and improve the quality of dry material. The temperature range used in the drying process, not exceeding + 30 ° C, provides optimal conditions for the preservation of biologically active substances in the product. Drying in a chamber under vacuum of frozen ground material is carried out at a pulsating pressure with a pulsation frequency of at least 10 Hz and an amplitude of pressure fluctuations of at least 0.5 mm Hg. Pressure pulsations in a vacuum drying chamber are created by dosed pulsed supply of air into it with a residual moisture content of not more than 3 wt.% And a frequency of not less than 10 Hz. In the process of drying the material, it is periodically exposed to vibrational vibrations with a frequency of 10-50 Hz. The formation of pressure pulsations in the drying chamber and the effect of vibrational vibrations on the material contributes to the intensification of the process of removing moisture from the material, which reduces the drying time by 3-6 times (RF patent No. 2163438, IPC A 01 N 1/02, publ. February 27, 2001).

The disadvantage of the prototype method is the complexity of the technology of drying and grinding the material to an ultrafine state, as well as the need to use a large number of complex energy-intensive technological equipment (a crusher, a vacuum chamber with equipment to create a vacuum and pulsating pressure, a vortex mill, a compressor, etc.).

The technical result of the proposed technical solution is to simplify the process of processing antlers into ultrafine powder and reduce the amount of complex energy-intensive equipment by combining the drying and grinding of frozen crushed material in a vortex mill while maintaining the biological activity of the final product.

The specified technical result is achieved by the fact that in the method of processing antlers of deer and reindeer into ultrafine powder, which includes cutting of antlers, freezing and crushing together with the skin or with hair and skin to particles no larger than 0.5 mm in size, drying the material, after which material is additionally crushed to particles with a size of 0.1-30.0 μm in a vortex mill, according to the invention, the drying of crushed frozen material is combined with its additional grinding in a vortex mill in a gas stream medium moisture content not exceeding 10 wt.% while maintaining the vortex mill automatic gas stream temperature not higher than + 50 ° C to give the finished soot from antlers having a non-radioactive carbon isotope ¹³ C in structure in an amount not less than 1.3 wt.% of carbon content in the finished product, which is a marker of the authenticity of the product. Moreover, the loading of the vortex mill with crushed frozen material is carried out cyclically with an interval between loading cycles sufficient for the output of the finished ultrafine antler powder of at least 70 wt.%.

The time of simultaneous drying and grinding of one portion of crushed frozen antler material between loading cycles does not exceed 1.5-5 hours.

Before additional grinding and drying of the frozen crushed antler material in a vortex mill, this material is pre-mixed with the finished ultrafine antler powder with the content of the latter in the mixture in an amount of at least 20 wt.%, Having a residual moisture content of not more than 10 wt.%.

As a gaseous medium, air, or nitrogen, or carbon dioxide, or argon, or helium is used.

After drying, the crushed material is Packed in a light-tight vacuum packaging. Such packaging prevents oxidative processes in the product and increases the shelf life of up to 2-3 years or more.

In accordance with the above, the set of essential features of the proposed technology for processing and preserving antlers in comparison with the set of essential features of the known technology-analogues meets the criteria of "novelty" and "inventive step", because allows you to get a product in a simpler way and with less energy-intensive technological equipment while preserving its biologically active substances and at the same time its conservation and processing.

Figure 1 shows a vortex mill, a General view; figure 2 is a section aa in figure 1.

Antlers processing technology

Example 1. Antlers of deer and / or reindeer are cut in the standard way, after which they are immediately placed in thermostat containers and frozen in the permafrost of the North, or in liquid nitrogen. If necessary (depending on the requirements for the final product), after short-term freezing, the skin of antlers is removed mechanically from the skin of the antlers and again placed in thermostat containers to completely freeze the material. In this form, antlers are stored for a long time or sent for processing.

Before drying, frozen antlers, together with the skin or with the hair and skin, are crushed using a standard bone crusher, rolling equipment, or using a cryogenic ball mill designed by NTK Flint in liquid nitrogen to a particle size of not more than 500 microns.

Further, the crushed and frozen material is dried and its grinding to an ultrafine state is carried out in a vortex mill developed by the Vortex Technology company, Novosibirsk (RF patent N 2057588, MKI B 02 C 19/06, published on 04/10/96) , which is a gas-dynamic grinder that uses the energy of compressed gas to accelerate the crushed particles of the product in a vortex stream. The vortex mill contains (Figs. 1 and 2) a housing 1 with inlet 2 and outlet 3 nozzles, an upper 4 and a lower 5 end caps, a central hole 6 in the upper end cap 4, an insert 7 with a profiled inner surface, with an entrance slit 8 and output classification slots 9, a loading vortex chamber 10 with a screw pipe 11 and a tubular feeder 12. A temperature sensor 13 is placed in the chamber, which is connected to the chilled gas supply valve 14 (inert or carbon dioxide, or air) through the pipe 15.

The process of drying and grinding frozen crushed material is as follows. An energy carrier compressed to 3-6 atmospheres gas (air, carbon dioxide, argon) with a moisture content of not more than 10 wt.% And a temperature of not more than 50 ° C, enters through the inlet pipe 2 and slot 8 into the vortex grinding chamber formed by insert 7 and end lids 4, 5. Crushed frozen material entering the tubular feeder 12, is drawn into the area of reduced pressure and reaches the grinding chamber. Further, the material is involved in the rotational movement and, under the action of centrifugal forces, is delivered to the profiled walls 7, where the particles of the material begin to intensively collide with each other and with the profiled walls 7, move along the path caused by the profiled walls, grind and dehydrate. The most suitable trajectory for dehydration and grinding is the polygon. A rotating gas-weighted flow forms in the chamber. Part of the gas, together with the finished product, leaves the chamber through outlet 9 into the housing 1 and pipe 3, and part with moisture vapor into the hole 6. The exhaust gas stream with moisture vapor exiting through outlet 6 enters the chamber 10, where it continues to rotate . Due to rotation in the center of this flow, a region of reduced pressure forms, which closes with a similar region in the grinding chamber.

In this case, the central hole 6 in the end cap 4 carries two fractions at once: in the central part of the hole 6, the mill is loaded with crushed frozen material, and at the periphery near the edge of the hole 6, the outlet of the spent moist energy carrier is released. The temperature in the grinding chamber is controlled by a temperature sensor 13. When the temperature of the gas flows exceeds + 50 ° C, valve 14 opens and cool dry gas (air, or inert or carbon dioxide) with a moisture content of not more than 10 wt.% Is supplied to the grinding chamber which reduces the temperature of the gas flows in the grinding chamber. Dehydrated and crushed material, reaching a particle size of not more than 1-30 microns and a moisture content of not more than 10 wt.%, Is discharged with a gas stream into the classification outlet 9 and pipe 3.

Crushed frozen material enters the tubular feeder 12 cyclically with an interval between loading cycles sufficient for the output of the finished ultrafine antler powder of at least 70 wt.%. The time of simultaneous drying and grinding of one portion of crushed frozen antler material between loading cycles does not exceed 1.5-5 hours, depending on the state of the starting material: particle size and their moisture content.

When loading through a tubular feeder 12, for example, 1 kg of crushed material with a moisture content of 67% by weight after 2 hours, 750 g of finished powder will come out of the nozzle 3 with a moisture content of 3.5 wt%, after which 1 kg of crushed material is again fed into the tubular feeder 12.

The antler powder has in its structure a non-radioactive isotope of carbon C ¹³ in an amount of not less than 1.3 wt.% Of the carbon content in the finished product. The obtained ultrafine powder from antlers is Packed in a light and gas tight vacuum packaging.

Example 2. The processing of deer antlers and / or reindeer, including their freezing, crushing and simultaneous grinding and drying, is carried out in accordance with example 1. In addition, before additional grinding and drying of the frozen crushed antler material in a vortex mill, the specified crushed and frozen material is preliminarily mixed with the finished ultrafine antler powder having a residual moisture content of not more than 10 wt.% and contained in the mixture in an amount of not less than 20 wt.%. As a rule, the ratio of crushed material with antler powder is from 5: 1 to 2: 1. After the moisture is equalized over the entire mass of the mixture, a tubular feeder 12 of the vortex mill is fed in portions (cyclically). At the same time, the grinding and drying time of crushed antler material is reduced by 1.5 or more times, which is advisable to apply for large volumes of production of ultrafine antler powder and the use of a high-performance vortex mill.

When loading through a tubular feeder 12, for example, 1 kg of crushed material pre-mixed with 20 wt.% Dry antler powder with a moisture content of 5 wt.% And a total humidity of 47% by weight after 1 hour 10 minutes, 720 g of finished powder with a moisture content of 3.0 wt.%, after which 1 kg of material mixture is again fed into the tubular feeder 12 for simultaneous grinding and drying.

Example 3. The study of the isotopic composition of carbon in ultrafine powder from antlers and the content of labile substances

Studies of the isotopic composition of carbon, C ¹² , C ¹³ antler powder, manufactured by the claimed technology, performed by mass spectrometry, electron impact. The sample was heat treated at t 650 ° C in an atmosphere of pure oxygen. The measurements were carried out on the peaks of CO ₂ . Atmospheric CO _{2 was} used as a reference.

Preliminary data showed that the carbon isotope composition (C ¹² ) is from 98.53 to 98.7%; (C ¹³ ) from 1.3 to 1.47% while the benchmark value of the laboratory’s ambient air corresponds to (C ¹² ) 98.9%; (C ¹³ ) 1.1% and is close to the natural composition.

Experimental studies have shown the beneficial effect of the non-radioactive isotope of carbon C ¹³ on body cells (Kaznacheev V.P., Rzhavin A.F., Mikhailova L.P. On the issue of thermonuclear bioenergetics of living matter // International Symposium "Cold Nuclear Fusion and New Energy Sources""(May 24-26, 1994). - Minsk, 1994. - p.190-195). With age or under the influence of adverse environmental conditions (the Far North, the Arctic, difficult working conditions), irreversible changes in the cells of human tissue structures occur due to a decrease or disappearance from the cells (for the reasons listed) of the carbon isotope 13, which is responsible for youth in the body and cell health. A person begins to weaken very quickly, grow old and often get sick. With the help of antler baths, antler cosmetics, C ¹³ isotopes penetrate the cells of the whole body through the skin and subcutaneous tissue, improving its general condition, enhancing protective functions, restoring energy, health and ensuring longevity. The proposed method of harvesting and preserving antlers allows you to save the carbon isotopes With ¹³ in the same state.

The proteins in the ultrafine powder obtained by the claimed method and the prototype method were determined by the chromatographic method, vitamins were determined by high performance liquid chromatography with the appropriate standards, and the hormone content was determined by radioimmunoassay (steroids were extracted from the powder with diethyl ether before determination).

Analysis of table 1 below shows that the inventive method of preserving and processing antlers with a simpler technology and with less equipment provides the same drying and grinding conditions as in the prototype method, which is confirmed by the content of labile substances (globulins, vitamins and hormones) in the same amount as in the ultrafine powder obtained by the prototype method. Moreover, the type of energy carrier has little effect on the content of labile biologically active substances in the finished product.

Table 1 Comparative data on the content of labile substances in ultrafine powder from antlers, prepared by the prototype method and the claimed method No. p.p. Indicators Prototype The inventive method air argon sour gas nitrogen one Protein, mg% 61200 61100 61190 61210 61240 The fractional composition of the protein,% 2 from the total amount: albumin 44 44.5 44.5 44.5 44.5 globulin 39 38.6 38.7 38.7 38.8 Vitamins, mg% 3 BUT 0.7 0.7 0.75 0.7 0.8 E 0.9 1,0 1,0 1,0 1,0 D 0.3 0.3 0.3 0.3 0.31 FROM 0.1 0.1 Hormones four Plasma growth hormone, ng / g 57.0 - - 58.0 58.5 Somatostatin, ng / g 11.0 - - 10.5 10.5 Insulin ng / g 10.7 - - 11.0 11.1 Testosterone ng / g 7.0 - - 6.7 7.0 Estradiol, ng / g 1.4 - - 1,5 1,5

Industrial applicability. The proposed technology for producing antler ultrafine powder can be applied both in large food or pharmaceutical complexes and in workshops of small firms with the appropriate equipment.

Claims (3)

1. A method of processing deer antlers and reindeer into ultrafine powder, including cutting antlers, freezing and crushing together with the skin or hair and skin to particles no more than 0.5 mm in size, drying the material and further grinding it to particles with a size of 0 , 1-30.0 μm in a vortex mill, characterized in that the drying of crushed frozen material is simultaneously combined with its additional grinding in a vortex mill in a gas stream with a moisture content of not more than 10 wt.% With automatic feeding Rye gas stream temperature is not above 50 ° C to give the finished soot from antlers having a non-radioactive carbon isotope ¹³ C in structure in an amount not less than 1.3 wt.% of the carbon content in the final product, and load the vortex mill crushed frozen material carried out cyclically with an interval between loading cycles sufficient for the output of the finished ultrafine antler powder of at least 70 wt.%, and the time of simultaneous drying and grinding of one portion of crushed frozen p Antovy material between loading cycles does not exceed 1.5-5 hours 2. The method according to claim 1, characterized in that before additional grinding and drying of the crushed antler material in a vortex mill, said material is pre-mixed with the finished ultrafine antler powder with a content of the latter in the mixture in an amount of at least 20 wt.%, Having a residual moisture content of more than 10 wt.%. 3. The method according to claim 1, characterized in that as a gaseous medium, air, or nitrogen, or carbon dioxide, or argon, or helium is used.

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