KR101445334B1 - Vegetable Soft Capsule Composition without Chemical Metal Salts - Google Patents

Abstract

The present invention relates to a vegetable soft capsule composition which does not includes chemical metal salts. More particularly, the content of iota carrageenan which is a high price vegetal gelating agent is less than 6 wt%. Chemical metal salts such as sodium salt and potassium salt are not used, but capsules are not crumbled, and soft capsules can be adhered only through pressure without heating. According to the present invention, the quantity of carrageenan which is 10-20 times more expensive than starches (starch or denatured starch) is minimized, so that costs spent to produce soft capsules can be saved. Sodium (salt) which is a chemical synthesized produce causing adult diseases such as hypertension and cardiac disorders is not used, and heat is not applied in an adhering (suturing) step, so that the heat denaturing of an active ingredient contained in the content of soft capsules can be prevented.

Description

[0001] The present invention relates to a vegetable soft capsule composition containing no chemical metal salt,

The present invention relates to a vegetable soft capsule composition which does not contain a chemical metal salt. More specifically, the present invention relates to a composition containing a chemical metal salt such as a sodium salt or a potassium salt by containing a small amount of less than 6% by weight of an iota- To a vegetable soft capsule composition capable of adhering a soft capsule with no pressure without heating, without disassembling the capsule without using a solvent.

In general, a soft gelatin capsule is prepared by mixing a certain amount of gelatin, glycerin, and water, and heating and dissolving the mixture at 70 to 80 ° C to prepare a coating solution. The characteristics of the coating solution form a gel-like film in a semi-solid state at a temperature of less than about 35 < 0 > C. A spreader box attached to a soft capsule molding machine flows the coating solution into a casting drum, and the casting drum rotates to form a thin film coating. At this time, the temperature of the casting drum is 15 DEG C or less, and a film (ribbon) having elasticity is rapidly formed as soon as the coating solution is closed on the casting drum. The formed ribbon passes through a transfer roller of a molding machine and passes through a die roll and a wedge (heat transfer device). The soft capsule molding machine is equipped with a casting drum and a spreader box on both sides so that the ribbons made on both sides are overlapped and passed between the two die rolls, And the soft capsule is adhered to the die by a die made on the die roll by using this principle. A certain amount of the contents passed through the urea just before the soft capsules are bonded is injected into the soft capsules sealed at the lower end, and the upper end is sealed to complete the molding of the soft capsules.

Most of the gelatin used in soft capsules is made by processing Cattle Hide, Cattle Bone and Pig skin. When the gelatin is dissolved in a certain amount of water, the solution has a thermoreversible property according to the temperature change. The thermoreversible property of a gelatin aqueous solution means that it is present in a viscous liquid colloid form (Sol) at high temperature and changed into a semi-solid form (Gel) at low temperature. Gelatin is used in most common soft capsules because it has these properties.

Recently, due to diseases of cattle and pigs such as mad cow disease and foot-and-mouth disease, social awareness of animal raw materials has deteriorated and research on plant materials has been continuously carried out. Also, in the case of gelatin, the process is often disgusted and unsanitary, and is often reported in the press. Gelatin is obtained by hydrolyzing collagen and has a structure in which amino acids are linked by a peptide bond and are entangled in a linear or complex branch shape. Due to this feature, in the case of soft capsules made of gelatin, disintegration is delayed due to the components such as aldehyde, tannin and limonene contained in the contents of the capsule, and the disintegration is delayed. When the content of the capsule is hard, And if the pH of the content is as low as 1.2 or less, there is a problem that the coating film is hydrolyzed to cause leakage (content leakage). Because of this, studies have been made for decades ago to manufacture soft capsules from natural-derived carbohydrate materials without using animal protein gelatin.

In order to overcome and replace the disadvantages of gelatin, which is an animal soft capsule material in the past, various kinds of garlic, pre-classified and carrageenan have been developed as vegetable soft capsule materials. Among them, carrageenan is classified as iota -, kappa - and lambda - carrageenan. In particular, in the case of iota carrageenan, calcium ion (Ca2 +) is required to form a gel network and sodium ion Na +) has been known to be required (WJ Reilly, 2002, Garrageenan)

A film forming composition comprising modified starch PCT / US2000 / 018420 (modified starch and Iota carrageenan and a process for producing a soft capsule using the same) is characterized by using modified starch and iota carrageenan as a film former, Sodium salt or potassium salt is used, the bonding temperature of the film is 25 to 80 DEG C, and the wet film has a melting point of 4 to 20 DEG C higher than the bonding temperature. It is expensive because of the high amount of carrageenan, which is high in viscosity and relatively expensive, because of the large amount of iota carrageenan added to the modified starch. In order to prepare a coating solution, it is heated to a temperature of 75 캜 or higher, and since the melting point of the produced wet film is 65 캜 or higher, the bonding temperature is actually 45 캜 or higher. In this case, since the injection wedge needs to be heated, the contents passing through the wetch will be affected by heat.

Application No. 10-2009-7020170 [Non-animal derived soft capsule shell and soft capsule with it] is characterized by containing lambda carrageenan, including sodium salt, and the adhesion (sealing) temperature is 30 to 40 degrees.

Application No. 10-2011-0036823 [non-animal soft capsule coating composition with improved cloudiness and film hardness] is characterized by inhibiting aging of starch by adding an antioxidant and a disintegration aid to inhibit disintegration stability and hardness increase , Organic acid metal salt as a buffer, and sodium phosphate dibasic acid, and the characteristics of carrageenan are not mentioned.

Application No. 10-2012-7015423 [film-forming composition for soft capsules] is characterized by the use of acid-degraded, lead-free, nongenic corn starch (acid-decomposed corn starch) having a specific viscosity at a certain temperature, There is no mention about it.

Most vegetable soft capsules use metal salts as buffers, mostly sodium salt forms. Medicines or health functional foods soft capsules consumed for health do not help promote public health. In addition, since the bonding temperature (sealing temperature) is very high, the contents to be filled in the soft capsule may cause heat denaturation. It is preferable to reduce the use amount of the carrageenan because the cost of the product increases as the use ratio of the expensive carrageenan is higher than the proportion of the modified starch. In addition, it is not desirable to use chemically synthesized products such as salts and buffers in order to approach marketing as a plant-derived soft capsule.

The inventors of the present invention have made extensive efforts to overcome the problems of the prior art, and as a result, they have found that when the amount of iota carrageenan is reduced, the manufacturing cost of soft capsules is lowered and sodium (salt) which adversely affects the human body is not used And that the non-animal-derived soft capsules which do not cause thermal denaturation of the contents due to a low adhesive (sealing) temperature can be produced. Thus, the present invention has been completed.

Accordingly, it is an object of the present invention to provide a non-animal-derived soft capsule which comprises a modified starch for film formation and a small amount of high-purity carrageenan for gelation, so that disintegration of the capsule is not required without using a metal salt such as sodium salt or potassium salt, The present invention is to provide a vegetable soft capsule composition which can adhere soft capsules only by pressure without heating and which is less economical than carrageenan.

According to one aspect of the present invention, there is provided a wet film composition for soft capsules comprising modified starch and iota-carrageenan, wherein the weight ratio of modified starch to iota-carrageenan is 4.1: 1 to 6.5: 1, The wet film composition for soft capsules is characterized in that it does not contain a buffer.

Conventionally, a soft capsule wet film composition comprising an iota-carrageenan (Korean Patent No. 10-0541722) contains a buffering agent which is a chemical metal salt and has a weight ratio of modified starch to iota-carrageenan of 1.5: 1 to 4.0: 1, Is characterized in that the weight ratio of modified starch to iota-carrageenan ranges from 4.1: 1 to 6.5: 1 and does not comprise a buffering agent which is a chemical metal salt. According to the experimental example of the present invention, when the weight ratio of the modified starch to the iota-carrageenan was not more than 4.0: 1, the disintegration time exceeded 20 minutes in the case where the weight ratio of the modified starch to the iota-carrageenan was 4.0: According to the present invention, when the weight ratio of modified starch to iota-carrageenan is set to 4.1: 1 or more, the disintegration time can be reduced to 20 minutes or less without containing a chemical metal salt buffer.

In the present invention, the modified starch may be any conventionally known modified starch capable of forming a soft capsule together with iota-carrageenan, and is preferably a hydroxypropylated corn starch or a hydroxypropylated tapioca starch By weight based on the total weight of the composition.

In the present invention, the above-mentioned iota-carrageenan may be any known iota-carrageenan in an average molecular weight range, and preferably has an average molecular weight of 400,000 to 600,000 DT. do. Analysis of the Iota-carrageenan used in the examples of the present invention by GPC chromatography revealed that the polymer had an average molecular weight of about 490,000 DT, a molecular weight of less than 15% and a molecular weight of 50,000 DT or less of 85% Or more.

In the present invention, the wet film composition for soft capsules is characterized in that the iota-carrageenan is contained at a concentration of 4 to 5.9 wt% based on the total weight of the wet film composition.

Conventionally, a soft capsule wet film composition comprising an iota-carrageenan (Korean Patent No. 10-0541722) contains 6-12% by weight of iota-carrageenan in the composition, whereas the wet film composition for soft capsules of the present invention contains iota-carrageenan Is contained in an amount of 4 to 5.9% by weight of the composition. According to the experimental example of the present invention, when the content of iota-carrageenan was not more than 6% by weight, the disintegration time exceeded 20 minutes but the content of expensive iota-carrynanan When the content of iota-carrageenan was reduced to 5.9% by weight or less, the disintegration time could be reduced to 20 minutes or less without containing a chemical metal salt buffer. Further, according to the experimental example of the present invention, it was confirmed that when the content of iota-carrageenan was set to 4% or more, the gelation in the aqueous solution became good.

In the present invention, there is provided a wet film composition for soft capsules, wherein the chemical metal salt is a sodium salt or a potassium salt. Conventionally, in the case of iota carrageenan, calcium ion (Ca 2+) is required to form a gel network and sodium ion (Na +) is required to disintegrate at 20 ° C (WJ Reilly, 2002, Garrageenan). However, in the present invention, for the first time, when the content of expensive Iota carrageenan is reduced, gelation is favorably performed without a chemical metal salt such as sodium salt or potassium salt, and it was first discovered that the disintegration time can be shortened to 20 minutes or less.

In the present invention, the wet film composition for soft capsules is characterized in that the disintegration time of the capsule is within 20 minutes at 37 ° C without using the chemical metal salt. It has been proved that the disintegration time of the capsules can be shortened to less than 20 minutes at 37 DEG C without using a chemical metal salt such as a sodium salt or a potassium salt when the content of the expensive Iota carrageenan is reduced. Disintegration time is defined as the time during which solid or solid formulations such as tablets and capsules dissolve in the test solution or disperse below the prescribed particle state, that is, the time during which the tablet or capsule is melted or dispersed in the stomach when ingested. It is stipulated in the Korean Pharmacopoeia and Health Functional Food Promotion Notified by the Safety Agency, and the capsules should be disintegrated within 20 minutes at 37 ℃ purified water.

According to the present invention, there is provided a wet film composition for a soft capsule, characterized in that the soft capsule can be adhered only at room temperature without heating the welle when the soft capsule is bonded. In an embodiment of the present invention. When the chemical metal salt was used for shortening the disintegration time, it was necessary to heat the weke temperature for adhesion of the capsule capsule to 50 degrees or more. However, when the content of the expensive iota carrageenan was reduced according to the present invention, And below) can be bonded by pressure only. The pressure of the wedge during the adhesion is in the range of 200 kPa to 500 kPa.

In the present invention, it is preferable to use a composition comprising 24.2 to 26% by weight of modified starch, 4 to 5.9% by weight of iota carrageenan, 15 to 25% by weight of a plasticizer, and 45 to 55% The present invention provides a wet film composition for soft capsules, which comprises purified water. The wet film composition of the present invention may further contain preservatives, coloring agents and the like, which are used in general soft capsules, if necessary.

In the present invention, the plasticizer may be any plasticizer used in conventional soft capsules, but preferably it is at least one selected from the group consisting of glycerin, D-sorbitol, sugar alcohols, and polyols To provide a wet film composition for capsules.

According to another aspect of the present invention, there is provided a dry film composition for soft capsules comprising a modified starch and an iota-carrageenan, wherein the weight ratio of modified starch to iota-carrageenan ranges from 4.1: 1 to 6.5: 1, Wherein the dry film composition for soft capsules does not contain a buffering agent for soft capsules.

In the present invention, it is preferable that the composition contains 48.4 to 52% by weight of modified starch, 8 to 11.8% by weight of iota carrageenan, and 37 to 43% by weight of a plasticizer, based on the total weight of the dry film composition A dry film composition for soft capsules is provided. The dry film composition of the present invention may further contain preservatives, coloring agents and the like, which are used in general soft capsules as necessary.

As used herein, the term " wet film composition for soft capsules " refers to a wet film composition supplied on a casting drum by mixing and dissolving the film raw materials for the production of soft capsules, in particular soft capsules prepared using a rotary die encapsulation device Quot; means a film composition in a dried state after the wet film composition is passed through a rotary die to form a filled capsule, followed by a drying process, and finally, a dry film composition for soft capsules. Water is removed from the wet film composition through the drying step, and the content of the composition in the composition is doubled as shown in Table 1 below.

Basic composition ingredient The weight percent of wet film composition The weight percent of dry film composition Modified starch 24.2 to 26 48.4 to 52 Iota carrageenan 4 ~ 5.9 8-11.8 Plasticizer 15-25 30 to 50 Purified water 45 to 55

Hereinafter, the present invention will be described more specifically.

It is an object of the present invention to be able to prepare soft capsules using plant-derived ingredients such as starch and carrageenan.

In order to solve the above problems, a plant-derived polymer capable of forming a film must first be selected. For this purpose, we investigated the properties of various cereals, documents, cellulose and its processed products (denaturation, decomposition, etc.) and selected raw materials effective for film formation.

It was confirmed that most unprocessed raw materials (pre-sorting, cellulose, etc.) do not form a film or that a physically very weak film is formed. It has been found that pre-processing grades facilitate film formation, especially corn-derived modified starches have high viscosity and good film formation upon dissolution. Therefore, the present inventor has continued research to apply a gelling agent having a thermoreversible property as a basic property in the production of a soft capsule.

Carrageenan is a plant-derived polymer that is known to have thermoreversible properties similar to gelatin. The kind of carrageenan which is effective for the film formation and the proper blending amount which does not cause a problem in film formation and does not cause disintegration are set.

Starch is used as a source of energy for human beings, such as cereals, corn, potatoes and sweet potato. The structure of starch can be divided into amylose and amylopectin. Generally, starch from grain is composed of 15 ~ 30% of amylose and 70 ~ 85% of amylopectin, but glutinous rice or waxy corn is amylopectin Most of them.

When hot water is poured into starch or suspended in water, the starch particles expand and become a viscous liquid, that is, a full state. This phenomenon is called luxury, but it can be seen in a certain temperature range depending on the type of starch. Amylose is linearly bound to glucose molecules, and when it is suspended in water, it warms up easily when heated, and forms a film upon drying after the gelation.

Modified starch is prepared by hydrolyzing starch or oxidizing and decomposing starch. Common modified starches are classified into acid-modified starches, oxidized starches, starch derivatives, alpha starch, ether starch, ester starch, soluble starch, crosslinked starch and grafted starch. Among these modified starches, ether starch has a strong stability against pH, is easy to be gelled, and has good film forming ability. In particular, the hydroxypropylenic group in which a hydroxypropyl group is ether-bonded is used as a film-forming agent of non-animal-derived soft capsules because it has a low initial initiation concentration and is non-ionic, has excellent aging stability, and can form a strong and elastic film.

Hydroxypropylated modified starches of starch from various grains were examined and corn - derived modified starch, which is composed of amylose and amylopectin, was selected as a film - forming agent for soft capsules. Hydroxypropyl corn starch is readily available from starch processing companies.

In order to produce a wet film for molding during the process of soft capsules, the coating solution must be gelled at a low temperature and therefore must have thermoreversible properties. Among the vegetable materials, carrageenan is known to be the only material with thermoreversible properties. Carrageenan is produced by extracting red algae such as Eucheuma cottonii, Eucheuma spinosum, and Chondrus crispus with water or alkali. Carrageenan is divided into Iota, Kappa, and Lambda carrageenan according to its structural characteristics, and the composition of these three carrageenans varies depending on the type of seaweed processed. The structural characteristics of carrageenan are distinguished by the degree of ester linkage of the sulfates and the composition ratio of 3,6-anhydrogalactose in the Galactose sugar unit. Iota carrageenan is composed of 32% Sulfate ester and 30% 3,6-anhydrogalactose, kappa carrageenan is composed of 25% Sulfate ester and 34% 3,6-anhydrogalactose and Lambda carrageenan is composed of 35% Sulfate ester 3,6-anhydrogalactose is not included. Due to these compositional characteristics, each carrageenan has different physico - chemical characteristics.

Kappa carrageenan can form thermoreversible gels in aqueous solution when potassium ion (K +) is present, iota carrageenan can form thermoreversible gels in aqueous solution, and when potassium ion (K +) or calcium ion (Ca + Or a gel having high strength can be formed. In case of lambda carrageenan, thermoreversible gel can not be formed. In the case of kappa carrageenan, it forms a hard and fragile gel, and in the case of Iota carrageenan, it forms a transparent and elastic gel. Since these gels formed from iota carrageenan and kappa carrageenan have a property of dissolving in water at 70 ° C or higher, they must be supplied with salt containing sodium. When the sodium salt is added, the coating preparation containing carrageenan is dissolved in water at 20 ° C.

Gel with iota carrageenan is a carrageenan that has the most suitable properties for non-animal derived gelatin-free soft capsules because of its excellent transparency and elasticity. [Gelatine Handbook, Theory and Industrial Practice by Reinhard Schrieber and Herbert Gareis, 2007, 3. Practical Aspects, 3.1.1.2 Carrageenans; Handbook of Pharmaceutical Excipients, Fourth Edition, Raymond C Rowe, 2003, Carrageenan]

Carrageenan is produced in a mixed form of Iota carrageenan, kappa carrageenan and lambda carrageenan according to the kind of algae and the extraction method. In recent years, separation purification technology has been developed, and products having a specific purity of carrageenan are being sold. In the case of iota carrageenan, the gelation properties are also different depending on the purity, and the gelation characteristics vary depending on the distribution of the molecular weight. The present inventors have found that high purity Iota carrageenan can form a solid gel at a low concentration, as a result of testing the gelation properties of standardized iota carrageenan, non-standardized iota carrageenan, and high purity iota carrageenan. In general, Iota carrageenan has an average molecular weight of about 100,000 to 10,000,000 DT. However, the Iota carrageenan used in the present invention is derived from Eucheuma spinosum or Chondrus crispus and has an average molecular weight of 400,000 DT ~ 600,000DT, less than 15% of low-molecular form of less than 50,000DT and more than 85% of polymer form of 50,000DT or more. In addition, the present invention is pure Iota carrageenan which has a purity of 100% and does not contain saccharides (sugar, glucose, maltodextrin, lactose) or metal salts (calcium, sodium) for controlling viscosity or jelly strength. In order to confirm the molecular weight distribution of Iota carrageenan of the present invention, it was confirmed by entrustment to the Korea polymer testing & research institute, an internationally recognized testing institute.

BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is an Iota carrageenan molecular weight analysis chart used in an embodiment of the present invention. Fig. According to the analysis chart, it can be confirmed that the average molecular weight (Mw) is 489,265 DT. As a result of the above experiment, it was confirmed that the distribution of each molecular weight was confirmed, and the molecular weight of less than 50,000 DT was less than 15%.

In the examples of the present invention, the amount of iota-carrageenan for gelation was determined by dissolving it by concentration, and after confirming the viscosity and the gelation state, it was confirmed that gelation occurred in an aqueous solution of 4% or more. If it is less than 4%, it remains in the Sol state even if it is cooled to 15 캜 or lower, and is present as a sticky, fluid liquid, so that the gel can not produce a wet film. On the other hand, an aqueous solution of 10% or more is highly viscous (over 10,000 cp at 80 ° C) and must be excessively heated in a soft capsule manufacturing process and spreading process for film dissolution process, transfer and film formation is very difficult This is an undesirable concentration.

The disintegration time of the Iota carrageenan gel was determined by concentration to confirm the dissolution properties of the capsules after the production of the soft capsules, that is, the effect on the disintegration. As a result, it was confirmed that the dissolution time increases with increasing concentration. In addition, it was confirmed that when the carrageenan was blended more than 6%, the disintegration criterion (37 ° C, within 20 minutes) was not satisfied when the wet film was prepared and dried with a certain concentration of iota carrageenan and modified starch. In addition, it was confirmed that disintegration time was shortened when sodium salt (sodium phosphate dibasic) was added, whereas disintegration time was delayed when potassium salt (potassium chloride) was added. This is proven by the fact that, in the case of iota carrageenan, as well as the sodium salt form, it does not dissolve well in cold water. In addition, it has been confirmed that sodium salt, which is generally used for buffering soft capsule, is used as an aid for disintegration. Some patents mention that potassium salts can be used for buffering, but this is not desirable because it causes a delay in disintegration.

As a result of the gel-forming properties and the effect on the disintegration of the Iota carrageenan by the concentration, it was confirmed that the film was formed at less than 6%, preferably 4.0% ~ 5.9% of the film dissolving solution, and no disintegration problem was observed without the sodium salt .

In order to confirm the relationship between the blending amount of iota carrageenan and the soft capsule sealing temperature, the film solution was prepared by concentration and the heating temperature (adhesion temperature) of the wetch was examined. As a result, the wet film produced at a concentration of less than 6% It was confirmed that the adhesive could be made only by the pressure of the molding die (mold) without the need. This is because some of the modified starch has sticky properties and can be adhered without the influence of carrageenan gel. In the case of most plant-derived soft capsules, the blending amount of carrageenan is large and the melting point of the wet film becomes high, so the temperature of the adhesive wette is set high. In this case, the contents of the capsule pass through the wetsy and are injected into the capsule, and some of the contents are returned to the contents tank, and the contents are continuously heated. Generally, when the contents are heated, the heat-sensitive components (saponin, some water-soluble vitamins, etc.) may cause a decrease in the content. In addition, in the case of the contents made of beeswax or PEG series suspending agent, layer separation occurs and undesirable properties may appear after the capsules are filled. In addition, since heat is not applied, it is very preferable from the viewpoint of energy saving.

Thus, the inventors of the present invention have solved the disintegration problem without using the sodium salt by using the content of iota carrageenan to a minimum, prevented the deterioration of the contents, and completed the plant-derived soft capsule having a great economical advantage .

It minimizes the amount of carrageenan which is 10 to 20 times higher than whole starch (starch and modified starch) to save the cost of manufacturing soft capsules, and it can be used as a chemical compound sodium salt that causes adult diseases such as hypertension and heart disease. And it is possible to prevent thermal denaturation of the active ingredient contained in the contents of the soft capsule because heat is not applied in the adhesion (sealing) process.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a GPC chromatogram showing the molecular weight of Iota carrageenan used in the examples of the present invention. FIG.
FIG. 2A is a photograph showing gelation state by the concentration of Iota carrageenan in the embodiment of the present invention. FIG.
FIG. 2B is a graph showing a change in viscosity and a gelable period according to the concentration of Iota carrageenan in the example of the present invention.
Figure 3 is a graph comparing the disintegration time with the concentration of iota carrageenan and the addition of salt in the examples of the present invention.
Fig. 4 is a photograph showing a capsule form when the adhesive (wette) temperature is formed at room temperature in the embodiment of the present invention.
5 is a photograph showing the state of the capsule after 20 minutes from the start of disintegration in the example of the present invention.

Hereinafter, the present invention will be described in more detail with reference to Examples. These embodiments are only for illustrating the present invention, and thus the scope of the present invention is not construed as being limited by these embodiments.

[Experimental Example 1]

To determine the amount of high purity iota carrageenan required for gelation to make the wet film, the viscosity and gelation state were confirmed after dissolving by concentration.

1) Preparation method: After adding 0.5g of carrageenan to a 250ml beaker, make 100g of purified water, stir it, raise the temperature to 80 ℃ and fully hydrate. The viscosity was adjusted to 0.5 to 13% by weight in the same manner at intervals of 0.5% by weight, and the viscosity and gelation state were confirmed.

2) Viscosity measurement method

(1) Viscometer: Brookfield DV-II +

(2) Conditions: LV3, LV4 (Spindle), 80 DEG C, 20 rpm

3) How to confirm the gelation state: Drop the hydrated solution into a stainless steel plate at about 10 ° C by about 3g. After curing for 10 minutes, when the reagent spoon is pressed and released about 2mm, the gel should not get on the spoon and the gel should not break.

Confirmation of viscosity and gelation status of Iota carrageenan concentration density(%) 0.5 One 1.5 2 2.5 3 3.5 4 4.5 Viscosity (cp) 40 70 150 300 370 450 570 860 1010 Gel state Bad Bad Bad Bad Bad Bad Bad Good Good density(%) 5 5.5 6 6.5 7 7.5 8 8.5 9 Viscosity (cp) 1340 1680 2150 2740 3800 4950 5400 6010 7450 Gel state Good Good Good Good Good Good Good Good Good density(%) 9.5 10 10.5 11 11.5 12 12.5 13 Viscosity (cp) 8900 11500 13400 17600 Over 20000 Gel state Good Good Good Good Good Good Good Good

2A is a photograph showing the gelation state of each concentration of iota carrageenan. As shown in the photograph of FIG. 2A, when the concentration of iota carrageenan is 4% or more, a gel free from deformation or cracking can be formed.

FIG. 2B is a graph showing a viscosity change and a gelable period according to the concentration of Iota carrageenan.

As a result of the above experiment, it was confirmed that gelation was obtained in an aqueous solution of 4% or more of Iota carrageenan. If it is less than 4%, it is in a state that it is sticky and easily crumbled in the state of Sol when it is cooled, so that it can not produce a wet film. On the other hand, an aqueous solution of 8% or more has a viscosity as high as 5000 cp or more, which requires excessive heating in the process of producing a soft capsule, and it is very difficult to perform a coating process for the dissolution process, transfer and film, to be.

[Experimental Example 2]

After the preparation of the soft capsules, the wet film was prepared by changing the concentration of the iota carrageenan in order to confirm the properties of dissolving the capsules in water, and the disintegration pattern was confirmed by drying. In general gelatin soft capsules, the amount of the powder component (gelatin) is about 40%. However, since the carrageenan of the present invention shows an abrupt viscosity by the low-temperature purified water, The amount should be about 30%. The plasticizer that imparts the elasticity of the film after drying is glycerin in the same manner as the gelatin soft capsule, and is set between 15 and 25 wt%, which is generally used amount. The purified water was set at about 45 to 55% by weight as a dissolving agent. Further, in order to confirm the effect of the potassium salt and the sodium salt, experiments were carried out by adding 1 wt% of potassium chloride and sodium phosphate to the comparative example of 7.5 wt% of Iota carrageenan, respectively.

1) Film production method: Weigh pure water, Iota carrageenan (corresponding weight%), hydroxypropyl corn starch and glycerin into a 250 ml sterilized glass bottle, and stir with a spoon for 5 minutes. The bottle cap is closed, immersed in a water bath at 80 ° C, and heated for 30 minutes to prepare a film solution. The film solution is made thin on a flat stainless steel plate to a thickness of about 0.8 mm. Transfer to a drying room (20 ~ 25 ℃, humidity 20 ~ 25%), dry for 1 day, and store at room temperature for 10 days.

2) Disintegration test method: The dried film was cut into 10 mm width and 10 mm length, placed in a disintegration test tube, and reciprocated to 37 ° C purified water to measure the disintegration time.

Disintegration pattern of Iota carrageenan concentration and effect of potassium and sodium salt Example 1 Example 2 Example 3 Example 4 Example 5 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Iota carrageenan (%) 4 4.5 5 5.3 5.9 6 7 7.5 7.5 Hydroxypropyl corn starch (%) 26 25.5 25 24.8 24.2 24 23 22.5 22.5 glycerin(%) 20 20 20 19.9 19.9 20 20 20 19.5 Purified water(%) 50 50 50 50. 50 50 50 50 49.5 Potassium chloride (%) One Sodium phosphate (%) Disintegration time (minutes) 11 13 15 16 19 21 24 30 47

3 is a graph comparing the disintegration time according to the carrageenan concentration and the addition of the salt.

From the above results, it was confirmed that the disintegration time of the film was increased as the blending ratio of iota carrageenan was increased. Further, it was confirmed that when the blending ratio was 6% or more, the disintegration standard (37 ° C, within 20 minutes) was not satisfied. In addition, the disintegration time was shortened in Comparative Example 5 in which a sodium salt was added, whereas in Comparative Example 4 in which a potassium salt was added, disintegration time was confirmed to be delayed. This is proven by the fact that, in the case of iota carrageenan, as well as the sodium salt form, it does not dissolve well in cold water. In addition, it has been confirmed that sodium salt, which is generally used for buffering soft capsule, is used as an aid for disintegration. Some patents mention that potassium salts can be used for buffering, but this is not desirable because it causes a delay in disintegration.

Considering the above-mentioned problems, the concentration of high-purity iota-carrageenan without disintegration is 6% or less (4 to 5.9% by weight) and 8 to 11.8% by weight when converted into a dry film Do.

[Experimental Example 3]

[Example 3], a composition containing 6% or more carrageenan [Comparative Example 1], and a composition using a sodium salt [Comparative Example 5] were used to confirm the blending amount of iota carrageenan and the sealing temperature of the soft capsule (Melting time, adhesion temperature) and the quality of soft capsules (disintegration, adhesion rate, bursting strength) were compared using a conventional rotary die molding machine.

1) Composition of coating solution

(1) Example 3: 5% by weight of iota carrageenan, 25% by weight of hydroxypropyl corn starch, 20% by weight of glycerin, 50%

(2) Comparative Example 1: 6% by weight of Iota carrageenan, 24% by weight of hydroxypropyl corn starch, 20% by weight of glycerin, 50%

(3) Comparative Example 5: 7.5% by weight of iota carrageenan, 22.5% of hydroxypropyl corn starch, 19.5% of glycerin, 49.5% of purified water, 1%

2) Manufacturing method

(1) Total weighing of each weight percentage corresponding to 100kg as seaweed.

(2) Add purified water and glycerin into a 400 L coating dissolution tank.

(3) Iota carrageenan and hydroxypropyl corn starch were added and stirred at 10 RPM for 10 minutes (Comparative Example 5 was added with sodium phosphate dibasic)

(4) Continue stirring and dissolve by raising the temperature to 80 캜 to 90 캜.

(5) Degrease at a vacuum degree of 640 mmHg or higher for about 10 minutes.

(6) Transfer to a thermostat container (receiver) and wait for molding.

(7) Use a soft capsule molding machine (Changsung, Jumbo Molding Machine) by using the film preparation and the contents (soybean oil).

(8) After drying for 3 days, store at room temperature for 20 days and conduct experiments.

Production conditions according to carrageenan concentration and soft capsule sealing temperature Example 3 Comparative Example 1 Comparative Example 5 Time required for film dissolution 30 minutes 40 minutes 45 minutes Coating fluidity (85 캜) Good Good Poor (high viscosity) Casting drum temperature 15 degrees 15 degrees 15 degrees Casting drum peeling Good Good Good Adhesion (Wetz) Temperature Room temperature (ungain) Room temperature (ungain) 52 ℃ Die pressure (kpa) 300 300 500 Adhesion rate 90% and 70% 70% and 50% 80% and 50% Tear strength (hardness 4N) 26 kg / cm ² 22 kg / cm ² 25 kg / cm ² Disintegration time (water, 37 ℃) 17 minutes 23 minutes 19 minutes

4 is a photograph showing a capsule shape when the adhesive (wette) temperature is formed at room temperature. As a result, it was confirmed that the capsules were not stitched in the case of Comparative Example 5 in which the content of iota-carrioni was high and the sodium salt was used.

5 is a photograph showing the state after 20 minutes from the start of disintegration. As shown in the photograph, in the case of Example 3 of the present invention and Comparative Example 5 using a sodium salt, the remaining amount of capsules is not visible on the disintegration assisting plate. However, in the case of Comparative Example 1 in which no sodium salt was used, much residue remained in the disintegration assisting plate even after 20 minutes.

As shown in the above results, in the case of Example 3, which is a composition of the present invention, molding was possible without applying heat at the time of bonding. In the case of Comparative Example 5 containing 7.5% of carrageenan, the bonding temperature was set to be very high (52 ° C) to confirm that molding was possible. In most plant-derived soft capsules, the blending amount of carrageenan is high, so that the melting point of the wet film is increased. Therefore, the temperature of the adhesive wette is set to be high, but when the composition of carrageenan is low, the hydroxypropyl corn starch has stickiness, It is judged that bonding can be carried out without being affected by the influence. In case of Comparative Example 1 containing 6% of Iota carrageenan, heat is not required for bonding, but disintegration time is not preferable to 23 minutes (within 20 minutes). As described above, when the amount of iota carrageenan was less than 6%, it was confirmed that the wet film could be adhered only by the pressure of the molding die (mold) without any heat, and that the disintegration stability was not affected without using the sodium salt.

As described above, according to the present invention, by using modified starch for film formation and a small amount of high purity carrageenan for gelation in the production of non-animal-derived soft capsules, disintegration of capsules can be achieved without using a metal salt such as sodium salt or potassium salt And the soft capsule can be adhered only by the pressure without heating, and the amount of the carrageenan to be used is less than that of the prior art, so that a vegetable soft capsule excellent in economy can be produced. In addition, it minimizes the amount of carrageenan which is 10 to 20 times higher than that of whole starch (starch and modified starch) to save the cost of manufacturing soft capsules, and is a chemical compound which is a chemical compound that causes adult diseases such as hypertension and heart disease ) Is not used and thermal denaturation of the active ingredient contained in the contents of the soft capsule can be prevented since heat is not applied in the adhesion (sealing) process.

Claims (11)

A wet film composition for soft capsules comprising hydroxypropylated corn starch or hydroxypropylated tapioca starch modified starch and iota-carrageenan, wherein the weight ratio of modified starch to iota-carrageenan ranges from 4.1: 1 to 6.5: 1 , And a buffering agent which is a chemical metal salt.
delete The wet film composition for soft capsules according to claim 1, wherein the iota carrageenan has an average molecular weight of 400,000 to 600,000 dt.
The wet film composition for soft capsules according to claim 1, wherein the iota-carrageenan is contained at a concentration of 4 to 5.9 wt% based on the total weight of the wet film composition.
The wet film composition for soft capsules according to claim 1, wherein the chemical metal salt is a sodium salt or a potassium salt.
The wet film composition for soft capsules according to claim 1, wherein the disintegration time of the capsule is within 20 minutes at 37 ° C without using the chemical metal salt.
The wet film composition for soft capsules according to claim 1, wherein the soft capsules can be adhered only at room temperature without heating the wetsy.
The composition of claim 1, wherein said wet film composition comprises 24.2 to 26 wt% modified starch, 4 to 5.9 wt% iota carrageenan, 15 to 25 wt% plasticizer, and 45 to 55 wt% The wet film composition for soft capsules according to claim 1,
The wet film composition for soft capsules according to claim 8, wherein the plasticizer is at least one selected from the group consisting of glycerin, D-sorbitol, sugar alcohols, and polyols.
A dry film composition for soft capsules comprising hydroxypropylated corn starch or hydroxypropylated tapioca starch modified starch and iota-carrageenan, wherein the weight ratio of modified starch to iota-carrageenan is 4.1: 1 to 6.5: 1, Characterized in that it does not comprise a buffering agent which is a chemical metal salt. delete

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