JPH0827035A - New powder collagen and its production - Google Patents

Abstract

PURPOSE:To obtain a new powder collagen excellent in touch feeling, having fine and uniform characteristics and useful in the fields of cosmetics, medicines, coatings, daily necessaries, foods, etc. CONSTITUTION:This powder collagen is obtained by controlling pH of a collagen solution in the vicinity of isoelectric point and subjecting the collagen solution to spraying and drying treatment (preferably at 80-85 deg.C) as an uniform dispersion in a concentration of 3-10%. The collagen solution is the aqueous solution of an soluble collagen and is obtained by using an alkali solubilizing method comprising deashing split leather after immersing leather to lime, adding a solution obtained by adding sodium sulfate to a mixed aqueous solution of sodium hydroxide with monomethylamine until the solution is saturated with sodium sulfate to the leather, stirring the mixture, carrying out alkaline treatment, neutralizing the solution, desalting the solution, crushing the treated leather, adding lactic acid to the crushed leather, kneading the crushed skin with lactic acid under stirring and filtering the kneaded product to afford Eucollagen. By controlling the collagen to the vicinity of isoelectric point, the collagen is deposited to give a dispersion in suspended state and the viscosity is lowered to enable spraying and drying in high concentration.

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to a powdered collagen used for various purposes in various industrial fields including cosmetics, pharmaceuticals, paints, etc., and particularly to a novel collagen having excellent tactile sensation, fine and homogeneous properties. The present invention relates to powdered collagen and a method for producing the same.

[0002]

BACKGROUND ART In recent years, in various fields such as cosmetics, pharmaceuticals, paints, daily necessities, and foods, attention has been focused on the usefulness of collagen powder for its various purposes. Particularly, it is excellent in touch, fine and homogeneous. There is a need for powdered collagen that has the property of being

Conventional methods for obtaining collagen powder include
1) A method of producing a collagen precipitate by adjusting the pH of a collagen solution to an isoelectric point, recovering the collagen precipitate, drying and then pulverizing the collagen powder (see Japanese Patent Publication No. 58-37330). 2) A method of obtaining collagen powder by spray-drying a collagen solution (JP-A-3-9-9).
No. 3716) are proposed.

However, since the method 1) above employs a mechanical crushing method, it has the drawback that the collagen may deteriorate due to the heat generated during crushing. Is difficult to obtain a homogeneous powder, and has a problem to be solved in terms of the feel of the product. In the method of 2) above, a normal collagen solution has a high viscosity, and it is difficult to bring a homogeneous spray state by spray-drying a high-concentration collagen solution. Although spray-drying is performed as a solution, this method has the drawback that it is difficult to obtain stable, homogeneous and high-quality powdered collagen, and the production efficiency is poor.

[0005]

DISCLOSURE OF THE INVENTION The present invention provides a novel powdered collagen having excellent texture and fine and uniform properties, and a method for producing the same.

[0006] That is, the present invention provides a powdered collagen produced by adjusting the pH of a collagen solution to near the isoelectric point and subjecting it to a spray dispersion treatment as a uniform dispersion at a concentration of 3 to 10%. It

The present invention will be described in detail below. The collagen solution which is the starting material of the present invention is an aqueous solution of soluble collagen, and the soluble collagen here means so-called soluble collagen such as acid-soluble collagen and neutral salt-soluble collagen, and so-called atelocollagen and eucollagen. It means general water-soluble collagen including solubilized collagen.

Of these, the solubilized collagen will be described as an example of the conventionally known method for producing solubilized collagen. Examples include animal-derived dermis, tendons, and rawhide, a by-product of the leather industry,
A method using proteolytic enzyme as a raw material such as floor skin after calcification (Japanese Patent Publication No. 44175/44, Japanese Patent Publication No. 44-110).
37) or a method of treating with an aqueous solution of caustic alkali and sodium sulfate (Japanese Patent Publication No. 46-15033).

Specific examples of production by the alkali solubilization method and the enzyme solubilization method will be given below. Alkali solubilization method (1) After the lime picking, the floor skin is decalcified and cut into 5 cm squares. 1 kg of the cut pieces of skin is taken, and a solution prepared by adding sodium sulfate to a 1N sodium hydroxide and 0.05M monomethylamine mixed aqueous solution until it is saturated is added at a liquid ratio of 1: 4. The temperature is adjusted to 25 ° C, stirred and treated for 10 days. After the treatment, 500 ml of hydrochloric acid is added to adjust the pH to about 4.8, and then 500 ml of a buffer solution is added to neutralize. Next, after washing with water and desalting, the skin is crushed with a wet crusher. The crushed skin is put in a kneading machine, lactic acid is added so as to be 1% of the total amount, and the mixture is kneaded and stirred at 10 ° C. for about 3 hours. The material thus obtained is filtered through a stainless mesh or the like to obtain eucollagen.

(2) The dermis layer of rawhide is taken out and made into a paste by a wet pulverizer. Take 1kg of the paste,
A liquid obtained by adding sodium sulfate to a mixed aqueous solution of 1N sodium hydroxide and 0.1M monomethylamine until it was saturated was added at a liquid ratio of 1: 5. Adjust the temperature to 25 ° C., stir and treat for 1 week. After the treatment, add 500 ml of hydrochloric acid,
The pH is adjusted to about 4.8 and then 500 ml of buffer is added to neutralize. This is washed with water and desalted, then placed in a kneader, lactic acid is added so as to be 1% of the total amount, and the mixture is kneaded and stirred at 10 ° C. for about 3 hours. Then, it is filtered through a stainless mesh to obtain eucollagen.

Enzyme solubilization method (1) The floor skin after the lime pickling is deashed and made into a paste by a wet pulverizer. Take 1 kg of the paste, adjust the substrate concentration to 2%, and adjust the pH to 3 with lactic acid. To this product, 1% of an acidic protease was added to the substrate, the temperature was kept at 25 ° C., and the mixture was kneaded and stirred in a kneader for 72 hours.
Then, it is filtered through a stainless mesh to obtain atelocollagen.

(2) The dermis layer of rawhide is taken out and made into a paste form by a wet pulverizer. Take 1kg of the paste,
Adjust the substrate concentration to 3% and bring the pH to 2 with acetic acid. 2% of acid protease to substrate
In addition, the temperature is kept at 25 ° C., and the mixture is kneaded and stirred by a kneader for 48 hours. Then, it is filtered through a stainless mesh to obtain atelocollagen.

In producing the powdered collagen according to the present invention, it is first necessary to use a collagen solution and adjust its pH to around the isoelectric point. Examples of the isoelectric point of the collagen solution are as follows. -Isoelectric point of alkali-solubilized collagen: pI = 4.5 to 5.0-Isoelectric point of enzyme-solubilized collagen: pI = 8.0 to 9.0

After the above collagen solution adjusted to near the isoelectric point was adjusted to a concentration of 3 to 10% with deionized water and stirred and dispersed using a homogenizer or the like to obtain a uniform dispersion liquid. , Spray-dry. The temperature conditions for spray drying can be raised within the range where collagen does not denature.

When the collagen solution is adjusted to have an isoelectric point, collagen is precipitated to form a suspension dispersion liquid, the viscosity of which decreases, and spray drying at a high concentration of 3 to 10% is possible. Become. In spray-drying the collagen dispersion adjusted to this isoelectric point, a homogenizer or the like should be used to thoroughly stir the solution to obtain a homogeneously dispersed solution. Needed above. When spray drying is performed in the state of a heterogeneous dispersion, the flow rate is not stable and it is difficult to form a uniform spray state, so stable, homogeneous and high-quality powder collagen is obtained. Is difficult.

As for the temperature condition for spray drying, in the case of the conventional collagen solution, the outlet temperature of the spray dryer is about 60 ° C. at the maximum, but as described above, uniform dispersion of a specific concentration adjusted near the isoelectric point is carried out. By subjecting the liquid to spray drying treatment, the thermal stability of collagen is increased, and by forming a homogeneous dispersion, a good spray state is formed. Can be raised. As a result, high-quality powdered collagen can be efficiently produced. However, depending on the device used for spray drying, any optimum condition can be selected depending on the concentration of the collagen dispersion or the amount of liquid to be sent.

According to the method of the present invention, since the product powder collagen has a uniform particle diameter and various conditions in the spray drying operation can be kept within a certain range, a stable spray drying treatment can be carried out. The effect is brought.

Hereinafter, the present invention will be described more specifically with reference to examples. Example 1 Using a 7% solution of eucollagen, its pH is adjusted to around the isoelectric point (pH = 4.8) with 1N-sodium hydroxide. The solution was diluted with deionized water to a concentration of 5% and then dispersed by stirring with a homogenizer to obtain a uniform dispersion. Using a spray dryer, this dispersion,
The hot air temperature and the liquid feed amount of the dispersion liquid were adjusted so that the outlet temperature was 80 ° C., and spray drying was performed to obtain uniform powder collagen having an average particle diameter of 19 μm.

When the powdered collagen obtained by this method was dissolved and the specific optical rotation was measured, [α] _D ²⁰ =
It was −410, which was a value specific to collagen, and no denaturation was observed.

Example 2 A 7% solution of atelocollagen was used and its pH was adjusted to about the isoelectric point (pH = 8.1) with 1N sodium hydroxide. The solution was diluted with deionized water to a concentration of 6% and then dispersed by stirring with a homogenizer to obtain a uniform dispersion. Using a spray dryer, this dispersion,
The hot air temperature and the liquid feed amount of the dispersion liquid were adjusted so that the outlet temperature was 80 ° C., and spray drying was performed to obtain uniform powder collagen having an average particle diameter of 20 μm.

The powdered collagen obtained by this method was dissolved and the specific optical rotation was measured. The filter [α] _D ²⁰ =-
It was 408, showing a value specific to collagen, and no denaturation was observed.

Example 3 Using a 10% eucollagen solution, its pH is adjusted to about the isoelectric point (pH = 4.8) with 1M sodium carbonate. This solution was diluted with deionized water to a concentration of 8% and then dispersed by stirring with a Dispers mill to obtain a uniform dispersion. This dispersion was spray-dried using a spray dryer while adjusting the hot air temperature and the amount of the dispersion to be fed so that the outlet temperature would be 85 ° C., to obtain uniform powdered collagen having an average particle size of 25 μm. It was

When the powdered collagen obtained by this method was dissolved and the specific optical rotation was measured, [α] _D ²⁰ =
It was −402, which was a value peculiar to collagen and no denaturation was observed.

Example 4 A 5% solution of atelocollagen was used, and its pH was adjusted to about the isoelectric point (pH = 8.3) with 1N sodium hydroxide. This solution was diluted with deionized water so as to have a concentration of 3%, and then dispersed by stirring with a dispers mill to obtain a uniform dispersion liquid. This dispersion was spray-dried using a spray drier by adjusting the hot air temperature and the amount of the dispersion to be fed so that the outlet temperature was 60 ° C., to obtain uniform powder collagen having an average particle size of 10 μm. .

When the powdered collagen obtained by this method was dissolved and the specific optical rotation was measured, [α] _D ²⁰ =
It was −400, which was a value specific to collagen, and no denaturation was observed.

The powdered collagen according to the present invention has a smooth uneven surface on the surface thereof, a soft tactile sensation, a fine structure and a uniform overall structure. On the other hand, the collagen powder obtained by spray-drying the collagen solution by the conventional method has no unevenness on the powder solid surface,
It has a solid feel. In addition, since the solid surface of the collagen powder obtained by the conventional pulverization method has irregularities, but has a sharp angle, the powdered collagen according to the present invention is extremely excellent in the sense of touch.

The powdered collagen according to the present invention has a large specific surface area of the powdered solid and has a proper hygroscopic property, and in use, when mixed with a liquid material or coated on the particle surface of a powdered material. In addition, the affinity with the object is significantly increased.

Claims (2)

[Claims] 1. A powdered collagen produced by adjusting the pH of a collagen solution to near the isoelectric point and subjecting it to a spray dispersion treatment as a uniform dispersion liquid at a concentration of 3 to 10%. 2. A basic solution is added to a high-concentration collagen solution to adjust the pH to near the isoelectric point, and deionized water is further added to obtain a solution having a concentration of 3 to 10%. A method for producing powdered collagen, which comprises subjecting the dispersion to spray drying.