KR20210030625A - Method for preparing amorphous granular starch using ethanol and high hydrostatic pressure - Google Patents

Abstract

The present invention relates to a method for manufacturing amorphous granular starch using ethanol and ultra-high pressure. A manufacturing method according to the present invention can manufacture amorphous granular starch, gelatinized starch, which is amorphous and has a granular structure, that is, the gelatinized starch that has lost its crystalline domain but retains its grain structure, inhibits swelling of starch by using ethanol, and induces a phenomenon that causes starch gelatinization by using ultra-high pressure, thereby having an effect of manufacturing edible amorphous granular starch without using a chemical method.

Description

Method for preparing amorphous granular starch using ethanol and high hydrostatic pressure}

The present invention relates to a method for producing amorphous particle starch using ethanol and ultra-high pressure.

Starch is a partially crystalline polymer having both a crystal region and an amorphous region. Starch exists in the form of particles and is a safe polymer that exists in nature, and is widely used in various industries, especially as a stabilizer and thickener in the food industry. However, when natural starch is used in industry, it has a limitation that it does not dissolve or disperse in water, so it is physically and chemically modified for various purposes.

Starch gelatinization refers to a process in which moisture is added to the starch and then heat is applied to the amorphous region, where hydration occurs first, expands, and accordingly, the crystal region is destroyed, the viscosity increases, and the particle shape is destroyed. In addition, at this time, a phase transition occurs in which the ordered structure in the starch particles changes to a disordered state, and the birefringence that occurs in natural starch is lost.

When natural starch is used in industry, it has a limitation that it does not dissolve or disperse in water, so it is physically and chemically modified for various purposes. Among these modified starches, alpha (α) starch (pre-gelatinized starch, instant starch) is an example of a starch whose properties of natural starch have changed due to physical changes. It is dehydrated starch. As a result, this starch is easily dispersed in cold water, and when water is added, it swells to a desired degree and the viscosity can be increased without heating. However, in the manufacture of gelatinized starch, when heat is applied to the starch, the shape of the particles is destroyed following the swelling of the particles, and at this time, there is a problem that the viscosity decreases rapidly and the water binding strength decreases.

To solve this problem, gelatinized starch having a particle structure was developed through chemical treatment, which is a method of chemically treating starch using an alkali solution or ammonia solution. Looking at their forms, they are gelatinized when compared to natural starch, but there is a possibility that a lot of changes in the shape of the particles occur and safety issues due to chemical treatment may be raised.

Accordingly, the present inventors confirmed that when preparing amorphous particle starch using ethanol and ultra-high pressure treatment, gelatinized starch having a particle structure similar to that of natural starch while having a fractured crystal region can be prepared, and completed the present invention.

Korean Patent Registration No. 10-0887699

It is an object of the present invention to provide a method for producing amorphous particle starch.

Another object of the present invention is to provide an amorphous particle starch prepared by the above manufacturing method.

Another object of the present invention is to provide a food composition comprising the amorphous particle starch.

Another object of the present invention is to provide a viscosity enhancer comprising the amorphous particle starch.

To achieve the above object,

The present invention comprises the steps of preparing a starch suspension by dispersing starch in an aqueous ethanol solution (step 1);

Subjecting the starch suspension of step 1 to ultra-high pressure (step 2);

Washing the starch by adding alcohol to the ultra-high pressure-treated starch suspension in step 2 and centrifuging (step 3); And

Drying and pulverizing the washed starch to obtain amorphous particle starch (step 4); Including,

The amorphous particle starch provides a method for producing amorphous particle starch, characterized in that the crystal region of the starch is lost, but the granular structure is maintained.

In addition, the present invention provides an amorphous particle starch prepared by the above manufacturing method.

Furthermore, the present invention provides a food composition comprising the amorphous particle starch.

Furthermore, the present invention provides a viscosity enhancer comprising the amorphous particle starch.

The manufacturing method according to the present invention can produce gelatinized starch that is amorphous and has a particle structure, that is, a gelatinized starch that has lost the crystal region of the starch but retains the particle structure, and uses ethanol to prevent the swelling of the starch. It has the effect of producing edible amorphous particle starch without using chemical methods by generating a phenomenon that causes starch gelatinization by using ultra-high pressure.

Figure 1 shows a method for producing amorphous particle starch using ethanol and ultra-high pressure of the present invention.
2 is a graph showing thermal properties of the amorphous particle starch of Examples 1 and 2 and the natural rice starch of Comparative Example 1 by DSC analysis.
3 is a microscopic analysis result of the amorphous particle starch of Examples 1 and 2 and the natural rice starch of Comparative Example 1. FIG.

Hereinafter, the present invention will be described in detail.

Method for producing amorphous particle starch

The present invention comprises the steps of preparing a starch suspension by dispersing starch in an aqueous ethanol solution (step 1);

Subjecting the starch suspension of step 1 to ultra-high pressure (step 2);

Washing the starch by adding alcohol to the ultra-high pressure-treated starch suspension in step 2 and centrifuging (step 3); And

Drying and pulverizing the washed starch to obtain amorphous particle starch (step 4); Including,

The amorphous particle starch provides a method for producing an amorphous particle starch, characterized in that the crystal region of the starch is lost but the particle structure is maintained.

In the production method of the present invention, step 1 is a step of preparing a starch suspension by adding an aqueous ethanol solution of 10 to 80% (v/v) to the starch, and the concentration of the aqueous ethanol solution is 10 to 30% (v/v). v) is preferable, and more preferably, a concentration of the aqueous ethanol solution of 20% (v/v) may be used.

The starch suspension may use 5 to 50 parts by weight of starch in 100 parts by weight of the starch suspension, more preferably 5 to 25 parts by weight. When the starch content in the starch suspension is less than 5 parts by weight, the concentration of the suspension is too low, and the efficiency is low, and when the content of starch exceeds 50 parts by weight, the transfer efficiency of ultra-high pressure decreases.

The starch is a natural starch obtained from plants, and examples of the starch include corn starch, tapioca starch, rice starch, potato starch, sweet potato starch, cassava starch, wheat starch, barley starch, sorghum starch, oat starch, rye starch, etc. May be, but is not limited thereto.

In the manufacturing method of the present invention, the step 2 may be performed by applying a pressure of 300 to 1,000 MPa, preferably, it may be performed by applying a pressure of 350 to 750 MPa, and more preferably, a pressure of 400 to 650 MPa. It can be done by adding. When the ultra-high pressure treatment pressure is less than 300 MPa, it is not sufficient to destroy the crystalline region of the starch, so that the ultra-high pressure treatment time is lengthened.

The ultra-high pressure treatment may be performed by applying ultra-high pressure for 10 to 60 minutes, preferably for 20 to 50 minutes, and more preferably for 30 minutes. If the ultra-high pressure treatment time is less than 10 minutes, it is difficult to prepare a completely amorphous starch, and if it exceeds 60 minutes, the process time is unnecessarily lengthened.

The ultra-high pressure treatment may be performed at 0 to 40°C, preferably at room temperature (25°C). When the ultra-high pressure treatment temperature exceeds 40°C, gelatinization of the starch occurs, and thus the particle structure is destroyed, making it difficult to manufacture an amorphous particle starch. In addition, when the temperature is out of the ultra-high pressure treatment temperature range, a separate cooling/heating device is required, thus unnecessarily increasing the process and increasing the cost.

In the production method of the present invention, in step 3, the starch suspension is subjected to ultra-high pressure treatment and then washed with alcohol. In this case, it is preferable to use centrifugation. Dehydration of the starch suspension is achieved through the above washing, and rapid sediment can be obtained by using centrifugation. The washing may be repeated a plurality of times, and the number of washings and rpm, temperature and time of the centrifuge may be appropriately determined according to the amount of alcohol used.

The alcohol may be a low-cost alcohol having 3 or less carbon atoms, such as methanol, ethanol or propanol, and preferably ethanol.

Amorphous particle starch

The present invention provides an amorphous particle starch prepared according to the above manufacturing method.

The amorphous particle starch refers to a gelatinized starch that has lost the crystal region of the starch but retains the particle structure. That is, the amorphous particle starch of the present invention is a processed starch in which the external shape of the natural starch is maintained, but the crystal region inside the starch particle is lost.

The amorphous form indicates that the crystalline region of the starch is lost, so that the starch no longer contains the crystalline region and has lost birefringence.

The particle structure refers to the appearance of grains, that is, granules, and the amorphous particle starch of the present invention maintains the shape of the grains, that is, the grain structure, like natural starch.

Food composition

The present invention provides a food composition containing the amorphous particle starch.

The food may be a health supplement, health food, health functional food, etc., but is not limited thereto. In addition, it includes adding the amorphous particle starch of the present invention to natural foods, processed foods, and general food materials.

Viscosity enhancer

The present invention provides a viscosity enhancer comprising the amorphous particle starch.

The viscosity enhancer may be used in food, chemical, industrial, and the like.

Hereinafter, the present invention will be described in more detail by the following examples. However, the following examples are merely illustrative of the present invention, and the contents of the present invention are not limited by the following examples.

<Example 1>

An aqueous ethanol solution of 20% (v/v) was added to 10 g of rice starch (based on the weight of solids) in consideration of the amount of moisture contained in the starch. At this time, a 10% (w/w) suspension was prepared by making the total of the suspension 100 g. The starch suspension was put into a plastic pouch pack, sealed, and shaken evenly. Thereafter, the plastic pouch pack containing the starch suspension was placed in an ultra-high pressure device (CIP Process controller, Ilshin Autoclave, Daejeon, Korea), and pressure was applied at room temperature (25°C) and 550 MPa for 30 minutes using distilled water as a pressure transfer medium. . After the ultra-high pressure treatment, the sample was immediately taken out of the plastic pouch bag, mixed with ethanol twice the volume of the suspension, and then centrifuged for 5 minutes at 3,000 rpm at 4° C. using a centrifuge. Washing was repeated by adding ethanol to the precipitate obtained by centrifugation again, and this was repeated two more times to wash a total of three times. Then, it was ^{dried in a 40 o} C dry oven for 24 hours, pulverized, sieved through a 100 mesh sieve, and passed through as a sample.

<Example 2>

An aqueous ethanol solution of 20% (v/v) was added to 15 g of rice starch (based on the weight of solids) in consideration of the amount of moisture contained in the starch. At this time, a 30% (w/w) suspension was prepared by making the total of the suspension 50 g. The starch suspension was put into a plastic pouch pack, sealed, and shaken evenly. Thereafter, the plastic pouch pack containing the starch suspension was placed in an ultra-high pressure device (CIP Precess controller, Ilshin Autoclave, Daejeon, Korea), and pressure was applied at room temperature (25° C.) and 550 MPa for 30 minutes using distilled water as a pressure transfer medium. . After the ultra-high pressure treatment, the sample was immediately taken out of the plastic pouch bag, mixed with ethanol twice the volume of the suspension, and then centrifuged for 5 minutes at 3,000 rpm at 4° C. using a centrifuge. Washing was repeated by adding ethanol to the precipitate obtained by centrifugation again, and this was repeated two more times to wash a total of three times. Then, it was ^{dried in a 40 o} C dry oven for 24 hours, pulverized, struck through a 100 mesh sieve, and passed through as a sample.

<Comparative Example 1>

Natural rice starch was prepared and used as Comparative Example 1.

Example Starch raw material Processing method Example 1 Rice starch 20% (v/v) ethanol aqueous solution added 10% (w/w) starch suspension preparation and ultra-high pressure treatment (550 MPa, 30 minutes), followed by ethanol washing Example 2 Rice starch 20% (v/v) ethanol aqueous solution added 30% (w/w) starch suspension preparation and ultra-high pressure treatment (550 MPa, 30 minutes), followed by ethanol washing Comparative Example 1 Rice starch -

<Experimental Example 1> Thermodynamic properties of starch

The thermodynamic properties of the amorphous particle starch of Examples 1 to 2 and the natural rice starch of Comparative Example 1 during gelatinization were measured. This was measured using a differential scanning calorimeter (Differential Scanning Calorimeter, DSC 4000, Perkin Elmar, Inc., Waltham, MA, USA) using the sealed empty pan as a reference. Examples 1 to 2 and Comparative Example 1 were prepared as suspensions having a moisture content of 75% (based on moisture). 15 mg of starch suspension was put in an aluminum pan and allowed to stand at room temperature for 1 hour to stabilize, then ^{maintained at 30 o} C for 1 minute, and then heated from 30° C. to 120° C. at 10° C./min to obtain a thermal characteristic curve. Got it.

As a result, as shown in FIG. 2, in the case of the natural rice starch of Comparative Example 1, a peak appears when the starch is gelatinized between 60°C and 73°C, and the gelatinization enthalpy (△H) value is 13.3J/g. have. However, in the case of Examples 1 and 2, the peak did not appear, and it was confirmed that gelatinization had already progressed and the crystal region inside was destroyed.

Onset (℃) Peak (℃) End (℃) Enthalpy (J/g) Example 1 - - - - Example 2 - - - - Comparative Example 1 60.6±0.1 67.5±0.2 74.6±0.4 13.3±0.7

<Experimental Example 2> Microscopic analysis of starch

Microscopic analysis of the amorphous particle starch of Examples 1 to 2 and the natural rice starch of Comparative Example 1 was performed. After dispersing by adding a small amount of distilled water to natural starch and amorphous particle starch, a drop was dropped on a slide glass, and a cover glass was covered to prepare a sample for analysis under a general optical microscope and a polarization microscope, and microscopic analysis was performed.

Specifically, the appearance was observed using unpolarized light by general optical microscopy analysis, and whether or not birefringence appeared through polarized light in a polarizing microscope was observed. In addition, in order to compare and observe the appearance of starch in detail, analysis was performed using a scanning electron microscope (Hiyachi TM3000, Tokyo, Japan). To this end, double-side carbon tape is attached to the aluminum stub, and natural starch and amorphous particle starch are scattered on it, and then gold powder is coated with a coating machine (MCM-200 Ion Sputter Coater) to avoid filling under the electron beam, and the image is 15 kV. Taken at an accelerating voltage of.

As shown in FIG. 3, in the case of the natural rice starch of Comparative Example 1, the particle shape can be confirmed (see FIG. 3 A1), and when viewing the B1 result observed with a polarizing microscope, it can be seen that the cross-shaped birefringence is clearly displayed. I can. In addition, the particle shape can be confirmed through the C1 result observed with a scanning electron microscope.

On the other hand, looking at the results of the amorphous particle starch (Examples 1 and 2), it was confirmed that the birefringence disappeared as a result of observation with a polarization microscope of B2 and B3, and it was found that gelatinization was achieved as in the DSC analysis result of Experimental Example 1. In addition, looking at the general micrographs of A2 and A3 and the scanning electron microscopy results of C2 and C3, it was confirmed that the starches of Examples 1 and 2 maintained the particle shape even though they were gelatinized.

So far, the present invention has been looked at around its preferred embodiments. Those of ordinary skill in the art to which the present invention pertains will be able to understand that the present invention may be implemented in a modified form without departing from the essential characteristics of the present invention. Therefore, the disclosed embodiments should be considered from an illustrative point of view rather than a limiting point of view. The scope of the present invention is not shown in the foregoing description, but in particular in the claims, and all differences within the scope equivalent thereto should be construed as being included in the present invention.

Claims (10)

Preparing a starch suspension by dispersing starch in an aqueous ethanol solution (step 1);
Subjecting the starch suspension of step 1 to ultra-high pressure (step 2);
Washing the starch by adding alcohol to the ultra-high pressure-treated starch suspension in step 2 and centrifuging (step 3); And
Drying and pulverizing the washed starch to obtain amorphous particle starch (step 4); Including,
The method for producing amorphous particle starch, characterized in that the amorphous particle starch is a gelatinized starch that has lost the crystal region of the starch but retains the particle structure.
The method of claim 1,
The starch suspension is characterized in that it comprises 10 to 50 parts by weight of starch based on 100 parts by weight of the starch suspension.
The method of claim 1,
The manufacturing method, characterized in that the ultra-high pressure treatment is performed by applying a pressure of 300 to 1,000 MPa.
The method of claim 1,
The ultra-high pressure treatment is a manufacturing method, characterized in that the ultra-high pressure is applied for 10 to 60 minutes.
The method of claim 1,
The manufacturing method, characterized in that the ultra-high pressure treatment is carried out at 10 to 40 ℃.
The method of claim 1,
The alcohol in step 3 is methanol, ethanol or propanol.
The method of claim 1,
The starch is a manufacturing method, characterized in that the natural starch obtained from a plant.
Amorphous particle starch prepared by the method of any one of claims 1 to 7.
A food composition comprising the amorphous particle starch of claim 8.
A viscosity enhancer comprising the amorphous particle starch of claim 8.

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