JP2002505263A - Non-viscous gel toothpaste - Google Patents

Abstract

  (57) [Summary] PROBLEM TO BE SOLVED: To provide a dentifrice which is surprisingly non-viscous and shows good consistency, transparency and physical stability. An orally acceptable medium, a brightener, a surfactant, and a binder, wherein the binder comprises kappa carrageenan and cellulose gum, wherein the concentration by weight of the binder is about 0.30-0.80. % And a ratio of kappa carrageenan to cellulose gum in the range of about 25: 75-75: 25.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

TECHNICAL FIELD OF THE INVENTION

The present invention relates to a gel dentifrice comprising kappa carrageenan and cellulose gum.
In particular, it relates to a gel dentifrice comprising a binder containing a cellulose gum such as carboxymethyl cellulose and kappa carrageenan in the formulation to provide a low stringency dentifrice. Dentifrice has good consistency and maintains good physical stability at relatively low concentrations of binder.

[0002]

2. Description of the Related Art

For the manufacture of dentifrice, the viscosity of the dentifrice ribbon is an important parameter that has been and continues to be of great interest. Large manufacturers generally have 8 per minute.
Fill the laminated tubes with dentifrice using a high speed filling line that can fill 0-200 tubes. To meet the demands of such production, it is important that the dentifrice ribbon be sharply cut from the tube. If the toothpaste remains on the sealing part of the laminated tube, the sealing of the tube is defective and
Create a gap in the tube. Also, the toothpaste ribbon coming out of the tube can cause blackening of the outer part of the tube in the sealing area due to burning while it is sealed. Tubes that have gaps and are blackened are discarded during manufacture. On the consumer side, viscous dentifrices give the dentifrice nozzle a shabby appearance when used. These problems are inherent in sagging or viscous dentifrices. In order to avoid or at least minimize these problems, a dentifrice formulation that results in a sharp cut, ie, a non-sticky or non-sticky dentifrice, is desired.

[0003] Dentifrices generally include brighteners or abrasives, wetting agents, thickeners or binders, water, foaming agents and perfumes. Wetting agents and water are also collectively referred to as media. In addition, agents that provide therapeutic or cosmetic benefits can be included, including, for example, fluoride and tartar control agents. To provide a non-sticky dentifrice, the formulation is:
Other good physical properties that consumers are accustomed to must be maintained. To satisfy consumers, these properties include attractive taste, good cleaning effect, easy rinsing, good mouth sensation, and even chemical and physical stability, Must be provided. Besides, toothpaste with these properties,
It must be low cost for consumers. The properties of dentifrice formulations depend on binders, abrasives, wetting agents, water and other inherent properties of the formulation, and they also determine how these components behave in complex mixtures with each other. Would depend on. In general, stickiness will be a function of the type and amount of binder and abrasive used in the dentifrice formulation. To a lesser extent, the viscosity will also be affected by the choice of wetting agent. Among the commonly used binders, for example, carboxymethylcellulose (CMC) generally promotes stickiness, while carrageenan is known to reduce stickiness. Among the commonly used abrasives, silica is generally chalk and dicalcium phosphate (DC
Increases stickiness compared to P).

[0004] The generic name carrageenan applies to many similar polysaccharides derived from seaweed. All carrageenans contain repeating galactose units linked by repeating β1 → 3 and α1 → 4 glycosidic bonds, and are partially sulfated. Carrageenan types can be distinguished in part by their degree of sulfation. Kappa carrageenan has a repeating unit of D-galactose-4-sulfate-4-sulfate-3,6-anhydro-D-galactose and has about 18
This results in a sulphate content of -25%. Iota carrageenan has repeating units of D-galactose-4-sulfate-3,6-anhydro-D-galactose-2-sulfate and provides a sulfate content of about 25-34%. Lambda carrageenan has a repeating unit of D-galactose-2-sulfate-D-galactose-2,6-disulfate and provides a sulfate content of about 30-40%.

[0005] Carrageenan forms a thixotropic gel. These gels are reported to exhibit excellent extrusion, perfume release and rinsing properties. The use of kappa and iota carrageenan as binders in gel dentifrices is also known to provide non-sticky dentifrices. However, U.S. Pat. No. 4,604,280 states that the problem with compositions made using carrageenan is that when the composition is subjected to mechanical work at a temperature lower than the gel sol temperature, the concentration or viscosity of the composition is reduced. It states that they are going down and winning. For carrageenan, the gel sol temperature is in the range of about 45-49 ° C. Sometimes less vigorous work at temperatures below this temperature substantially reduces the viscosity. To compensate for such a loss of viscosity, it is often necessary to use additional amounts of carrageenan in the formulation than is necessary. For that reason, carrageenan is often used at a weight concentration of 1% or more.

[0006] Among the types of iota, kappa and lambda carrageenans used in dentifrice formulations, iota carrageenans are commonly used. This choice is due in part to differences in curing effects. Compared to gels based on iota carrageenan, gels based on kappa carrageenan are reported to harden more easily during storage. Toothpastes that cure in this manner are difficult to squeeze from the tube. Also, compared to the iota type, gels based on kappa carrageenan have the problem of syneresis, i.e. they are more likely to separate water from the gel. Dentifrice products appear unacceptable if they are not stable to such phase separation. For these reasons, if carrageenan is used as a binder in gel dentifrices, the choice is usually of the iota type. It is an object of the present invention to provide a non-sticky gel dentifrice containing kappa carrageenan as a major component of the binder, without the aforementioned stability problems associated with kappa carrageenan. It is a further object of the present invention to provide a dentifrice having a relatively low concentration of kappa carrageenan.

[0007]

[Means for Solving the Problems]

It has been found that a binder comprising kappa carrageenan and cellulose gum in a dentifrice formulation provides a dentifrice that is surprisingly non-viscous and exhibits good consistency and physical stability. Dentifrice can also be formulated to have excellent transparency. The concentration by weight of binder in the formulation ranges from about 0.30-0.80%. The weight ratio of kappa carrageenan to cellulose gum in the binder is about 25: 75-
75:25. The preferred concentration of binder is in the range of about 0.45-0.65, and the preferred ratio of kappa carrageenan to cellulose gum is about 55
: 45-75: 25. A preferred cellulose gum is carboxymethyl cellulose (CMC).

[0008] The present invention comprises a binder comprising kappa carrageenan and cellulose gum in a formulation that is non-viscous, has good consistency, clarity, and exhibits good physical stability. About toothpaste. The present invention overcomes the stickiness problems associated with cellulose gums such as carboxymethylcellulose or CMC, and the syneresis and stability problems associated with kappa carrageenan. The binder obtained by mixing the cellulose gum and kappa carrageenan can be used in standard gel dentifrice formulations, is non-sticky, stable for long time separation of water and fragrance, has good Cuban Provides a dentifrice that has value (has good consistency) and does not harden significantly over time. Binders are useful at relatively low concentrations, which is important in terms of cost.

The present invention comprises an orally acceptable medium, a brightener, a surfactant, and a binder, wherein the binder comprises kappa carrageenan and cellulose gum, wherein the concentration by weight of the binder is about 0.30- A dentifrice composition is provided that is in the range of 0.80% and the ratio of kappa carrageenan to cellulose gum is in the range of about 25: 75-75: 25. Important features of the present invention are (a) the concentration by weight of binder, and (b) the weight ratio of kappa carrageenan to cellulose gum in the binder. Preferred concentrations of the binder are in the range of about 0.45-0.65%. A more preferred concentration of binder is about 0.4
5-0.61%. The preferred ratio of kappa carrageenan to cellulose gum is:
It is in the range of about 55: 45-75: 25. A more preferred ratio is about 60: 40-
75:25, an even more preferred ratio is about 62: 38-71: 29. The cellulose gum and kappa carrageenan in the binder are in the form of an anhydrous blend mixture or a mixture that has been treated together, both of which are suitable. These mixtures can be prepared according to methods generally known to those skilled in the art.

[0010] Cellulose gums that can be used by this method include those that are generally suitable as gum thickeners for dentifrices. Examples of these gums are hydroxyethylcellulose, hydroxypropylcellulose, and carboxymethylcellulose. As used herein, the term "cellulose" means any one or a combination of cellulose gums. A preferred gum is carboxymethylcellulose. Dentifrices usually include a medium, a brightener, a binder and a surfactant or detergent. In addition, agents that provide a therapeutic or cosmetic benefit, such as enamel hardeners, tartar control agents, whitening agents and antibacterial agents can be included. One or more sweeteners and flavoring agents are optionally added to satisfy the consumer. Titanium dioxide can also be added as an opacifying or whitening agent when such is desired. The dentifrice medium is an orally acceptable medium and includes water and a humectant, such as a 3-6 carbon polyol in which each carbon is hydroxylated, and mixtures thereof. Examples of humectants include glycerol, sorbitol, polyethylene glycol, polyoxyethylene glycol, mannitol, xylitol, and other sugar alcohols. Sorbitol and glycerol (glycerin) are preferred.

[0011] Brighteners or abrasives suitable for the dentifrices of the present invention include finely divided, water-insoluble powdered materials, many of which are well known to those skilled in the art. These materials have the activity of producing gloss instead of being overly abrasive. Examples include dicalcium phosphate, tricalcium phosphate, sodium metaphosphate, crystalline silica, colloidal silica, aluminosilicate complexes, calcium carbonate, magnesium carbonate, magnesium phosphate, calcium pyrophosphate, bentonite, talc, calcium silicate, aluminate Includes calcium, aluminum oxide and silica zero gel. Preferred abrasives are silica-containing abrasives.

The surfactants (detergents) that can be used in the dentifrices of the present invention are those that are commonly used to emulsify or otherwise evenly disperse the dentifrice components. It is generally preferred that the detergent is anionic or nonionic or a mixture thereof. Suitable types of anionic detergents are sodium lauryl sulfate, fatty acid monoglyceride sulfate, aliphatic alkyl sulfates, higher alkyl aryl sulfonates, higher alkyl sulfoacetates, higher olefin sulfonates, higher aliphatic acyl amides of lower aliphatic aminocarboxylic acids, higher aliphatic acyl amides, Alkyl poly lower alkoxy (3-100 alkoxy groups) sulfates, and fatty acid soaps. Examples of these anionic detergents are sodium lauryl sulfate, sodium hydrogenated coconut oil fatty acid monoglyceride monosulfate, sodium N
-Lauroyl sarcoside, and sodium cocaate. A preferred type of nonionic detergent comprises a chain of lower alkylene oxides, such as ethylene oxide and propylene oxide.

[0013] Additional substances that are optionally added include perfumes, enamel hardeners, and antimicrobial compounds. Examples of flavoring agents include the sweetening agents saccharin, essential oils such as spearmint, peppermint, peppermint, eucalyptus, lemon and lime. Examples of curing agents include sodium monofluorophosphate, sodium fluoride and tin fluoride. Examples of antibacterial agents are sodium benzoate and methyl or ethyl paracept. The dentifrice of the present invention can be manufactured as opaque or transparent. Without the addition of an opacifier, the dentifrice has good transparency. Titanium dioxide is a preferred opacifying agent, which can be added to provide an opaque dentifrice without affecting the physical properties of the formulation.

The dentifrice of the present invention can be manufactured in a manner well known to those skilled in the art. An example of a general approach performed at ambient temperature is as follows. The binder is dispersed in the sorbitol or glycerin by high speed stirring and the dispersion is stirred at that speed for 5 minutes. Water is added and the resulting gum slurry is stirred for a further 15 minutes. Separately, the anhydrous blend mixture is
Produced from sodium saccharin and sodium benzoate. If sodium fluoride, sodium monofluorophosphate, titanium dioxide or any other salt is used, they are added to the mixture at this stage. The mixture is then dispersed in the gum slurry and stirred with low agitation for 10 minutes to form a gel. Add colorant and mix by stirring for 5 minutes. The gel was then transferred to a Ross ™ mixer. Add silica and mix for 15 minutes under partial vacuum (at least 720 mmHg). Flavor was added and mixed for 10 minutes under full vacuum, then sodium lauryl sulfate was added and mixing continued for 15 minutes under full vacuum.
At this point, a sample was removed for testing and filled into a tube from the batch. The following examples illustrate, but do not limit, the invention.

[0015]

【Example】

Comparisons were made among a number of formulations with varying amounts of kappa carrageenan and CMC. Components other than the binders of kappa carrageenan and CMC were kept constant to evaluate the effect of the binder on the viscosity, Cuban value and stability. Table 1 shows the components that were constant in one set of comparisons.

[0016]

[Table 1]

Table 2 shows the varying amounts of kappa carrageenan and CMC containing the ingredients of Table 1
3 shows some of the formulations containing

[0018]

[Table 2]

* Iota carrageenan content is about 90-100%. The formulation produced by Iota Carrageenan contains 0.03% potassium chloride.

Test Results For each of the manufactured formulations, the viscosity, Cuban value and physical stability were measured. The viscosity of the formulation was measured using a texture analyzer. The texture analyzer has a plunger that moves down and touches a sample of the dentifrice. The plunger remains on the sample for the scheduled time and then only moves upwards, lifting the dentifrice ribbon with it. After the plunger has reached a certain height or distance with its upward movement, the dentifrice ribbon will break. The test stops as soon as the ribbon breaks and the distance (mm) traveled by the plunger is a measure of stickiness. The following is the detailed procedure used to measure stickiness for the present invention. A 2 g sample of dentifrice was placed in the center of the plate below the texture analyzer. The plunger force was set to 200 g and the pre-test speed of the plunger was set to 1 mm / sec. The pre-test speed is the speed at which the plunger moves down before the test begins. The plunger sample retention time was set at 2 seconds. This causes the plunger to touch the sample on the holding plate and remains there for 2 seconds before moving up. After the test,
It was set to 1 mm / sec. This is the speed at which the plunger moves upward.
The test is stopped as soon as the ribbon breaks and the distance traveled by the plunger (
mm).

The Cuban test value is directly related to the dentifrice viscosity. Cuban test (
Or, also referred to as the "Rack" test), the dentifrice is squeezed out of the tube through a fixed orifice through a grid of spaced parallel bars. The results of the test are displayed as the maximum number of intervals (number 1-12) indicating the longest distance between the bars that support the dentifrice ribbon without cutting it. The rack is about 300 mm long and about 100 mm wide. The stainless steel rod is 3 between rods 1 and 2.
The distance between the rods increases by 3 mm from rod to rod for the first time starting from mm (the number of intervals is 1). Therefore, the distance between rods 2 and 3 is 6 mm and 12
The th and thirteenth bars (the number of intervals: 12) are 39 mm. 1-2 and 9-12
Are unacceptable, 3 and 8 are acceptable, and 4-7 is good.

The stability test was performed by filling a tube with the sample paste. The tubes were capped and stored flat at room temperature and 50 ° C. for 12 weeks. After 12 weeks, a dentifrice ribbon approximately 5 cm long was squeezed out of the tube. The tube was then opened and the ribbon and contents evaluated for scent and phase separation (syneresis). Separation of the scent and aqueous phase at the tip of the dentifrice tube is recorded as a "wet cap". Scent separation is rated 0 = none, 1 = slight, 2 = moderate, and 3 = significant. Stability is rated as "not ok", "ok" and "good".
In order to be rated "not ok", a sample must have some undesirable properties, such as fragrance separation, syneresis, being very hard in a tube or having unacceptable Cuban values. It will be shown. "No problem (ok
) "Means that the sample did not separate but was somewhat granular and lacked good shine. To be rated as "good", the sample did not show any kind of separation and the sample was excellent with subtle details, such as fine texture, or not granular and had a good shine or gloss Will be. Table 3 shows the results of the Cuban value and stability tests for the formulations described above in Tables 1 and 2.

[0023]

[Table 3]

Item 1-8 in Table 3 shows that the ratio of kappa carrageenan to CMC is 52: 48−
Kappa carrageenan / CMC formulation ranging from 71:29. As can be seen from Table 3, Cub for kappa carrageenan / CMC formulation (items 1-8)
The an value is that the concentration by weight of kappa carrageenan is greater than 0.30% and that
When it is less than 50%, it is good. At higher concentrations of kappa carrageenan,
Thickening can also be a problem over time. Items 9-14 in Table 3 are representative of attempts to make suitable binders by mixing kappa and iota carrageenan. As can be seen from the Cuban values and / or stability results, these formulations are generally unacceptable. Item 15 in Table 3 is a representative example of an unsuccessful attempt to produce a suitable binder by mixing kappa carrageenan and xanthan.

In addition to providing a kappa carrageenan-containing gel dentifrice having good viscosity and stability, a further object was to provide a dentifrice that is also non-sticky.
As used herein, the term "non-sticky" means a dentifrice having low stickiness (less than about 20 mm). Certain gel dentifrices containing a binder comprising kappa carrageenan and CMC have been found to exhibit surprisingly low viscosity. To provide a dentifrice with low viscosity, the preferred weight percent concentration of the binder is about 0%.
. It is in the range of 45-0.61%. Within this range, Kappa Carrageenan vs CM
The preferred ratio of C is in the range of about 62: 38-71: 29. Table 4 shows how some representative dentifrices of the present invention are compared to other dentifrice formulations, including some widely used commercial brands. The formulation of items 1-22 comprises:
This is described above in Tables 1 and 2.

[0026]

[Table 4]

The dentifrices of the present invention (shown in Table 4 by items 1 and 2) have very low stickiness. The viscosity of these dentifrices is substantially lower than three of the four commercial dentifrices tested, and certain dentifrices of the present invention have significantly lower viscosities than the best commercial products tested. It has quality. Low viscosity was achieved with formulations using relatively low amounts of kappa carrageenan in the gel, showing good consistency and stability.

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Claims (12)

[Claims] 1. An orally acceptable medium, comprising a brightener, a surfactant, and a binder, wherein the binder comprises kappa carrageenan and cellulose gum, wherein the concentration by weight of the binder is about 0.30-0. A dentifrice composition wherein the dentifrice composition is in the range of 80% and the ratio of kappa carrageenan to cellulose gum is in the range of about 25: 75-75: 25. 2. The composition of claim 1 wherein the cellulose gum is carboxymethyl cellulose. 3. The composition of claim 1 wherein the concentration of the binder is in the range of about 0.45-0.65%. 4. The composition of claim 3, wherein the concentration of the binder is in the range of about 0.45-0.61%. 5. The composition of claim 5 wherein the ratio of kappa carrageenan to cellulose gum is about 55: 45-
2. The composition of claim 1 in the range of 75:25. 6. The ratio of kappa carrageenan to cellulose gum is about 60: 40-
6. The composition of claim 5 in the range of 75:25. 7. The ratio of kappa carrageenan to cellulose gum is about 62: 38-
7. The composition of claim 6 in the range 71:29. 8. The concentration of kappa carrageenan in weight percent of about 0.30-0.45.
The composition of claim 1, wherein the concentration of the cellulose gum is in the range of about 0.10-0.25. 9. The composition of claim 8 wherein the concentration of kappa carrageenan is in the range of about 0.32-0.38% and the concentration of cellulose gum is in the range of about 0.13-0.23%. 10. The composition of claim 1, wherein the abrasive is a silica-containing abrasive. 11. The composition according to claim 10, wherein the humectant is sorbitol, glycerin or a mixture thereof. 12. The composition of claim 11, further comprising titanium dioxide.