KR20130078411A - Preserved agents derived from plant resources for gelatin and gelatin made by using the same - Google Patents

Abstract

PURPOSE: A gelatin preservative solution using vegetable materials is provided to provide gelatin with reduced material property degradation and deterioration by microorganisms. CONSTITUTION: A gelatin preservative solution contains hydroxypropyl methylcellulose phthalate (HPMCP) and a base. 5-10 parts of base by weight are mixed with 100 parts HPMCP by weight. 1/160-1/6 of HPMCP is used for the weight of gelatin. The base is one or more compounds selected from a group consisting of NaOH, KOH, and Ca (OH)2. HPMCP contains 20-24wt% of methoxy substituent, 6-10wt% of hydroxypropoxy substituent, and 21-35wt% of phthalic acid, and the viscosity of the HPMCP is 48-66 cst. Gelatin is obtained by gelating and drying a HPMCP- gelatin solution.

Description

Preserved agents derived from plant resources for gelatin and gelatin made by using the same}

The present invention relates to a preservative solution and a gelatin prepared therefrom which enhances its preservation in order to provide a gelatin suitable for use in the food and medicinal field.

Gelatin has been used in a wide range of fields in food, medicine and industrial applications. The manufacturing process of gelatin for use in the food or pharmaceutical field is largely divided into three steps: a solution process for dissolving in hot water, a gelation process for gelling the solution at room temperature, and a drying process after gelation. However, gelatin is easy to be contaminated by microorganisms under various environments, and is difficult to apply to food or pharmaceutical fields due to the rapid deterioration of physical properties such as viscosity and gel strength.

In particular, gelatin in the solution process of the process is very vulnerable to microorganisms, and has a problem that the physical property change is very large. Because of this, care must be taken not to contaminate the microorganisms in the solution process, but gelatin begins to hydrolyze and generate microorganisms after about two days at a high temperature, and the viscosity decreases rapidly and a bad odor occurs.

In addition, even after gelation of gelatine to prepare a jelly form, it can be visually recognized that bacteria grow on the upper layer of the jelly from about one week later, and the jelly layer and the water layer are separated and odor starts to occur. After about two weeks, the gel appears to loosen, and the odor is very bad.

As such, gelatin begins to be contaminated by microorganisms when stored for two days or more in the manufacturing process, and gelatin intrinsic properties are lost.

In order to solve the above problems, various preservatives and preservatives have been used for a long time, but there is a limit in practicality due to a weak usage limit and microbial control function. In other words, the effect is insignificant, and it is known that there is no microbial control effect when used for a long time. In addition, there are not many preservatives that can be used in the food and pharmaceutical fields.

The present invention seeks to provide a preservative solution that improves the preservation of gelatin for use in the food and pharmaceutical fields. In addition, the preservative solution is used to provide a gelatin that is prevented from being deteriorated by microorganisms and reduced physical properties during storage.

The present invention includes hydroxypropyl methyl cellulose phthalate (HPMCP) and a base, the base is used in 5 to 10 parts by weight based on 100 parts by weight of hydroxypropyl methyl cellulose phthalate, the hydroxypropyl methyl cellulose phthalate is gelatin weight It provides a gelatin preservative solution, characterized in that it is used in a ratio of 1/160 to 1/5.

Preferably, the base is at least one selected from the group consisting of NaOH, KOH and Ca (OH) ₂ .

Preferably, the hydroxypropyl methyl cellulose phthalate is 20 to 24% by weight of methoxy (methoxy) substituent content, 6 to 10% by weight of hydroxypropoxy substituent (hydroxypropoxy) content and 21 to 35% by weight of phthalic acid (phthalic) acid) and has a viscosity of 48 to 66 cst.

The present invention is the step of swelling the gelatin preservative solution by mixing gelatin of 5 to 160 times with respect to the HPMCP weight And dissolving the swollen gelatin at a temperature of 60 to 80 ° C. to produce an HPMCP-gelatin solution. It provides a method for producing gelatin.

Preferably, the preservative solution is dissolved by dissolving 5 to 10 parts by weight of the base in water with respect to 100 parts by weight of HPMCP, and then mixed and dissolved by adding HPMCP at a ratio of 1/160 to 1/5 by weight of gelatin, and at room temperature It is prepared by storage for 12 to 24 hours.

The present invention provides gelatin obtained by gelling and drying the prepared HPMCP-gelatin solution.

According to the present invention, while maintaining or improving the physicochemical properties of the gelatin, it is possible to prevent the microbial deterioration and degradation of the gelatin during storage. Therefore, the present invention can be advantageously used in a wide range of fields in which gelatin is used, such as food, medicine, and industrial fields.

The present invention relates to a gelatin preservative solution which is vulnerable to contamination during storage and improves the preservation of gelatin, which rapidly decreases physical properties such as viscosity and gel strength.

The preservative solution is characterized in that it comprises hydroxypropylmethylcellulose phthalate (HPMCP) and a base. Specifically, the preservative solution of the present invention is prepared by the following method in one embodiment in the form of an aqueous solution comprising hydroxypropylmethylcellulose phthalate (HPMCP) and a base:

5 to 10 parts by weight of base is first dissolved in water and then mixed and dissolved by adding HPMCP to 100 parts by weight of HPMCP. Mechanical agitation is performed for 40 minutes to dissolve the HPMCP. After dissolution of HPMCP, the solution is stored at room temperature for a day to remove bubbles to obtain a clear solution of preservative solution.

The amount of HPMCP used in the preservative solution is preferably in a ratio of 1/160 to 1/5 of the gelatin weight. When using the HPMCP at a ratio higher than the above range, when the HPMCP-gelatin solution to be described below has a high viscosity above a suitable level and is applied to film forming, a problem occurs that the film is rough and brittle, and the HPMCP is used at a ratio lower than the above range. In case of gelatin, the preservation effect does not appear to be satisfactory.

As the base contained in the preservative solution, at least one selected from the group consisting of NaOH, KOH and Ca (OH) ₂ is preferably used. The base serves to help dissolution in dissolving HPMCP. That is, the base neutralizes HPMCP and easily dissolves in the aqueous system. When using a base of a high concentration exceeding the above range, there is a possibility that the preservative solution itself becomes alkaline.

The HPMCP, which is used as a main component of the gelatin preservative solution in the present invention, is a polymer used as a pharmaceutical coating and capsule, and is a derivative of cellulose, which is a major component of the plant cell wall. Therefore, the preservative solution provided by this invention is vegetable.

Specific examples of HPMCP include HPMCP HP-55 ^® (Samsung Fine Chemical Co., Ltd., methoxy content: 18-22%, hydroxy propoxy content: 5-9%, phthalic acid content: 27-35%, 200731 Type, viscosity range: 32-48 cst), HPMCP HP-55S ^® (Samsung Fine Chemicals, methoxy content: 18-22%, hydroxy propoxy content: 5-9%, phthalic acid content: 27-35%, 200731 Type, viscosity range: 136 ~ 204cst) and HPMCP HP-50 ^® (Samsung Fine Chemical Co., Ltd., methoxy content: 20 ~ 24%, hydroxy propoxy content: 6 ~ 10%, phthalic acid content: 21 ~ 27%, 220824 Type, viscosity range: 44-66 cst). The content of the substituent including methoxy represents the ratio of the sum of the atomic weights of the elements constituting the substituents to the sum of the atomic weights of the elements constituting the repeating unit of the substituted cellulose in the structure of Formula 1 below.

The HPMCP has different physicochemical properties according to each substituent content and molecular weight, and in the present invention, preferably 20 to 24% by weight of methoxy substituent, 6 to 10% by weight of hydroxypropoxy substituent and Hydroxypropylmethylcellulose phthalate having a phthalic acid content of 21 to 35% by weight and a viscosity of 48 to 66 cst is used.

The present invention provides a method for preparing gelatin having improved preservation using the preservative solution.

Specifically, the present invention comprises the steps of preparing a gelatin preservative solution containing hydroxypropylmethylcellulose phthalate; Mixing and swelling 5 to 160 times gelatin with respect to the weight of hydroxypropylmethylcellulose phthalate contained in the preservative solution and dissolving the swollen gelatin at a temperature of 60 to 80 ° C. to prepare HPMCP-gelatin solution. Characterized in that it comprises It provides a method for producing gelatin.

The amount of gelatin mixed in the preservative solution in the step of preparing the HPMCP-gelatin solution is preferably 5 to 160 times the weight of the HPMCP by mixing the gelatin in an amount greater than 160 times the weight of the HPMCP as described above. This is because when the final product is less antimicrobial, when mixed in less than 5 times the viscosity of the solution increases the problem that the final product breaks well when forming the film.

The "swelling" refers to a phenomenon in which gelatin absorbs and swells water, which is a solvent, and appears when a polymer material is dissolved. In other words, the polymer in the solid state has a strong interaction between the chains constituting the structure, but when it is immersed in the solvent, solvent molecules are interrupted between the polymer chains to swell into a gel, followed by a polymer chain surrounded by the solvent molecules. These are separated and dissolved in the solvent one by one, which is called swelling. In the step of swelling the gelatin of the present invention, the quantitated gelatin is added to an aqueous solvent and stirred, and then preferably left at room temperature for 30 minutes.

In addition, the preparation of the HPMCP-gelatin solution in the present invention corresponds to the "solution process" during the entire process of gelatin preparation, and subsequently the HPMCP-gelatin solution prepared above is the same as that performed in the normal gelatin preparation process. The gelation and drying process can be performed to produce gelatin with improved shelf life. In one embodiment, the gelling process is carried out by cooling the HPMCP-gelatin solution prepared above for 17 hours at a temperature (about 10 ℃) lower than the gelling composition, that is, the gelling start temperature of gelatin, the drying process is the gelling solution The film is cast in the form of a film using a caster it is carried out by drying for 24 hours at 25 ℃, 50% RH conditions.

Since the gelatin of the present invention improves the preservation by using the cellulose derivative of the vegetable component as the main component of the preservative solution, it is particularly advantageous to be included in foods and pharmaceuticals.

The present invention will be described in detail through the following examples.

Example  One

● Preparation of Preservative Solution

In addition to the gelatin and hydroxypropyl methyl cellulose phthalate (HPMCP) described in Table 1 below, NaOH was added and dissolved in water in an amount of 6.5% by weight relative to HPMCP. In this case, mechanical agitation was performed for 5 minutes using a mechanical stirrer. Then hydroxypropyl methyl cellulose phthalate (HP-50 ^® Samsung Fine Chemicals) was added to 0.1% by weight based on the preservative solution, mixed for 30 minutes to dissolve. In this case, mechanical agitation was performed for 40 minutes using a mechanical stirrer. After dissolution of HPMCP, the prepared sample was stored at room temperature for about a day to obtain a clear solution solution without bubbles.

● Gelatin-HPMCP Solution Preparation

To the prepared preservative solution was added gelatin having a strength of 200 bloom (manufactured by Geltech, B-type) to 16% by weight relative to the preservative solution and then swelled. In the swelling step, the gelatin quantified was added to an aqueous solvent, stirred using a water spoon, and left to stand at room temperature for 30 minutes as it is. The swollen gelatin was put into a water bath at 60 ° C. for 30 minutes and dissolved to obtain a gelatin-HPMCP solution.

Example  2 to 8

A preservative solution and a gelatin-HPMCP solution were obtained in the same manner as in Example 1 except that the amounts of gelatin and HPMCP for the preservative solution were as shown in Table 1 below.

Example  9

Gelatin (manufactured by Geltech, B-type) and hydroxypropylmethylcellulose phthalate (HP-55 ^® Samsung Fine Chemicals) with a strength of 250 bloom is used in amounts of 30% by weight and 0.5% by weight, respectively, based on the preservative solution. A preservative solution and a gelatin-HPMCP solution were obtained in the same manner as in Example 1.

Example  10 and 11

Gelatin (manufactured by Geltech, B-type) and hydroxypropylmethylcellulose phthalate (HP-50 ^® Samsung Fine Chemicals) having a strength of 200 bloom is used, except that the preservative solution is used in the amounts shown in Table 1 below, respectively. In the same manner as in Example 1, a preservative solution and a gelatin-HPMCP solution were obtained.

Comparative example  One

A gelatin aqueous solution containing a gelatin (B-type, manufactured by Geltech) having a strength of 200 bloom at a concentration of 16 wt% was prepared.

Comparative example  2

A preservative solution and a gelatin-HPMCP solution were obtained in the same manner as in Example 1 except that HPMCP included in the preservative solution was used in an amount of 0.05% by weight relative to the preservative solution.

*% By weight of gelatin and hydroxypropylmethylcellulose phthalate is% by weight relative to the preservative solution.

[Property evaluation]

● storage of prepared solutions

Gelatin-HPMCP solution or gelatin aqueous solution prepared in Examples and Comparative Examples were stored for 4 days in a thermostat maintaining 43 ℃.

The antimicrobial, apparent and fragrance grades of the solution were then evaluated after 1, 2, 3 and 4 days, and the change was assessed by measuring the initial and 4th day viscosity of the solution.

Antimicrobial Evaluation

<Total Aerobic Microbial test & Total Yeasts and Molds test>

After 1, 2, 3 and 4 days, 10 ml of the sample is taken from the solution, mixed with 90 ml of sterile saline solution, and diluted by decimal dilution method (10 ^-2 , 10 ^-3 , 10 ^-4). ..) 1 ml each (samples) were aseptically taken into two sterile petri dishes of 9-10 cm in diameter and 1.5 cm in height. After aseptically dispensing 15ml of the standard agar medium maintained at about 43 ~ 45 ℃, the sample and the medium was mixed well while rotating gently and tilted left and right while being careful not to attach to the petri-dish lid. Then cooled and solidified.

Next, 5 ml of standard agar medium was added again to prevent the occurrence of diffusion colonies. At this time, the time until the sample was taken and the medium was added did not pass more than 20 minutes.

Cooled and coagulated petri-dish was inverted (lid down) and incubated at 35 ± 1 ° C. for 36 hours. The medium was dried during culturing so that the weight was not reduced by more than 15%.

Immediately after incubation, colony counts were calculated using the colony calculator. Colony counts were calculated using a plate that had no diffusion colonies (less than half the petri-dish total area) and produced 30 to 300 colonies per plate (petri-dish). When 300 or more colonies were generated in all plates, the closest one was 300, and the lowest dilution factor was obtained when only 30 or less colonies were obtained for all plates. The number of bacteria in 1 ml of the sample is multiplied by the number of colonies in one plate by a significant dilution factor to clarify that it is a measure of colonies developed from certain restricted ones, and the value is multiplied by the number of bacteria in 1 ml (in 1 g). Listed. The results are shown in Table 2 below.

No growth was observed in the gelatin-HPMCP solution of Examples, but Comparative Example 2 containing the HPMCP contained in Comparative Example 1 or the preservative solution without using the preservative solution of the present invention in an amount less than the range defined in the present invention. In the case of it was confirmed that the growth of the bacteria starts from the third day.

Appearance and fragrance evaluation

After 1, 2, 3 and 4 days, the solution was visually observed and compared by odor. It was graded as follows.

(Double-circle): When the state of a solution does not show a noticeable change compared with the initial stage of manufacture, and there is no big difference with an initial state also in a fragrance characteristic.

○: The state of the solution is not a significant difference in apparent characteristics such as color, presence and degree of flow, viscosity (viscosity), and transparency compared to the initial stage of manufacture, but there is a slight change. If smells are mixed

◇: The condition of the solution has a noticeable difference in color, presence and degree of flow, viscosity (viscosity), transparency, etc. compared to the initial state of manufacture.

(Triangle | delta): When the state of a solution is discolored and deteriorated so that the initial manufacturing state cannot be found, the characteristics, such as the flowability and transparency, are also completely changed, and there is a very bad smell

The results are shown in Table 3 below.

Viscosity Change Assessment

Viscosity was measured by the following method after the initial and 4 days of the solution to evaluate the change.

Measuring instrument: BROOKFIELD Viscometer LV DV-11 + Pro

Measurement Condition: Speed (100rpm), Spindle (S61)

The results are shown in Table 3 below.

In the gelatine-HPMCP solution of Example, there was no change in appearance and flavor grade over time, but in Comparative Example 1 in which the preservative solution of the present invention was not used, from day 2, the HPMCP was less than the range defined by the present invention. In the case of Comparative Example 2, which contains a quantity, a decrease in the apparent and flavor grades occurred from the third day. In addition, the viscosity change was particularly improved in the example solutions compared to Comparative Example 1 in which no preservative solution was used at all.

From the above results, it can be seen that the addition of a preservative solution containing HPMCP has an antimicrobial effect and can continuously maintain the physical properties and quality of gelatin. In particular, as an example of the physical properties of gelatin, as the degree of change becomes more severe, the internal molecular structure itself or the intermolecular force between them is greatly affected, and the phenomena decrease gradually. In the case of applying the preservative solution of the present invention, It was confirmed that the change in the viscosity measurement occurred relatively slowly.

In addition, the higher the concentration of HPMCP contained in the preservative solution, the higher the antimicrobial and quality (physical) preservation effect.

Therefore, the preservative solution of the present invention including HPMCP functions to improve the physical properties of gelatin vulnerable to microbial deterioration while maintaining or improving the physicochemical properties of gelatin, thereby enabling a wide range of applications of gelatin in the food or pharmaceutical field.

Claims (6)

Hydroxypropylmethylcellulose phthalate (HPMCP) and a base,
The base is used in 5 to 10 parts by weight based on 100 parts by weight of hydroxypropyl methyl cellulose phthalate, the hydroxypropyl methyl cellulose phthalate is gelatin preservative, characterized in that used in a ratio of 1/160 to 1/5 to the weight of gelatin solution. In claim 1,
The base is a gelatin preservative solution, characterized in that at least one selected from the group consisting of NaOH, KOH and Ca (OH) ₂ . In claim 1,
remind Hydroxypropylmethylcellulose phthalate contains 20-24% by weight of methoxy substituent content, 6-10% by weight of hydroxypropoxy substituent content and 21-35% by weight of phthalic acid content. Gelatin preservative solution having a viscosity of 48 ~ 66cst. The gelatin preservative solution of any one of claims 1 to 3 mixed with swelling gelatin of 5 to 160 times the weight of the HPMCP by swelling And dissolving the swollen gelatin at a temperature of 60 to 80 ° C. to produce an HPMCP-gelatin solution. Method for producing gelatin. 5. The method of claim 4,
The preservative solution is dissolved in 5 to 10 parts by weight of a base in 100 parts by weight of HPMCP in water, then mixed and dissolved by adding HPMCP at a ratio of 1/160 to 1/5 by weight of gelatin, 12 to 24 at room temperature Characterized in that it is manufactured by storage Method for producing gelatin. Gelatin obtained by gelling and drying the HPMCP-gelatin solution prepared in claim 4.