NL8802460A - PACKAGED TOOTHPASTE. - Google Patents

Description

* 1 VO 1289

Packaged toothpaste.

The present invention relates to a toothpaste packed in a plastic laminate tube, mechanical dispenser, flexible packaging and the like. More particularly, it relates to a toothpaste 5 which is in compatible contact with a polyolefin surface of a package, such as a plastic laminate toothpaste tube, mechanical dispenser or flexible package.

For many years, toothpastes have been packaged in flexible metal tubes such as wax coated lead tubes, uncoated aluminum tubes or aluminum tubes with an epoxy resin coating on them. In recent years, flexible form-retaining laminated plastic tubes have become increasingly used.

Laminated plastic toothpaste tubes generally comprise an inner polyolefin resin layer which is in direct contact with the toothpaste and at least one intermediate layer including an aluminum foil layer which prevents taste loss of the toothpaste. Preferably, a paper intermediate layer is also provided, which provides stiffness to the tube. The outer layers are generally of polyolefin resins, one of which may be white colored and may contain printed indicia with a clear polyolefin laminate overcoat to protect the indicia.

Additional flexible plastic laminate interlayers may also be provided.

Mechanical toothpaste dispensers may also have a polyolefin surface that is in contact with the toothpaste contained therein. In fact, the polyolefin itself can be the housing of the device. Flexible bag-shaped packages can also have a polyolefin surface that is in contact with toothpaste.

Toothpastes typically contain a liquid carrier consisting of water and a wetting agent, a gelling agent solid carrier and a water-insoluble dental polishing agent.

"86024ÊO

-2-

A surfactant is also generally included. Toothpastes composed of such materials, the humectant comprising glycerine and sorbitol and the polishing material being an alkaline earth metal salt, such as dicalcium phosphate, have been successfully packaged in flexible metal toothpaste containers, including uncoated aluminum tubes, or having an inner coating of a epoxy resin enamel coating. However, it has been observed that when such toothpastes are otherwise packaged in containers with an internal polyolefin surface, such as plastic laminated toothpaste tubes, mechanically operated toothpaste dispensers or flexible bag-shaped packages, syneresis becomes a problem and liquids separate from the solid substances which make the toothpaste undesirable.

Applicant's previous patent applications have described additives for preventing toothpaste syneresis on contact with a polyolefin surface, for toothpastes containing alkaline earth metal phosphate or alpha-alumina trihydrate polishing agent. These patent applications are: Serial No. 771,378, Aug. 30, 1985, wherein the anti-syneresis additive for alkaline earth phosphate toothpaste is a polyethylene glycol; 25 U.S. Serial No. 803,040, November 27, 1985, wherein the anti-syneresis additive for an alpha alumina trihydrate toothpaste is a polyethylene glycol; U.S. Serial No. 808,755, December 13, 1985, wherein the anti-syneresis toothpaste additive with polishing agent is an alkaline earth metal phosphate propylene glycol; U.S. Serial No. 922,872, October 31, 1986, as "contilatio-in-part" of the now-expired application 808,756, December 13, 1985, wherein the anti-syneresis additive for a toothpaste having a polishing agent as a substantially an alkaline earth metal phosphate is an alkyl parahydroxybenzoate ester; * «-3- U.S. Serial No. 821,566, January 22, 1986, wherein the anti-syneresis additive for an alpha alumina trihydrate toothpaste is a vegetable oil; U.S. Serial No. 821,567, January 22, 1986, wherein the anti-syneresis additive for an alkaline earth metal phosphate toothpaste is a vegetable oil; and U.S. Serial No. 835,014, February 28, 1986, wherein the anti-syneresis additive for a toothpaste having polishing agent is primarily alpha alumina trihydrate benzoic acid. In each of the above patent applications, condensates of ethylene oxide with propylene glycol, ie, "Pluronic" materials, have generally been disclosed as a type of surfactant material which may be present in the various toothpastes described in the anti-syne. additive.

Japanese Patent Publication No. 75410/85 to Ebine et al (Lion Corporation) discloses a toothpaste in which glycerin is the only humectant, or is mixed with another humectant, such as sorbitol, but which glycerine is at least present in an amount of more than 20 wt. % of the toothpaste, since smaller amounts would result in unwanted evaporation of water if the toothpaste is packaged in a container with a plastic container body, at least the container portion of which has a water permeability of at least 5 g / m. day.50 you.

The high glycerin toothpaste is formulated to avoid evaporation and weight loss in this particular type of container. The description includes a general indication that a polymer of ethylene oxide and propylene oxide can be used as a surfactant.

U.S. Patent 4,556,553 to

Siganuma et al (Lion Corporation), discloses toothpastes containing an aluminum oxide abrasive in a container with an oxygen permeability of at least 3 cc / m. Day.atm in which the antiseptic properties are enhanced by .8802410-4- the presence of polyhydric alcohol comprising a mixture of sorbitol and glycerine. This is a general indication that condensates with ethylene oxide with propylene oxide can be used as a surfactant in the alumina toothpastes. Some toothpaste samples have been described for comparative purposes, containing dicalcium phosphate with sodium lauryl sulfate as the sole surfactant.

Japanese Patent Publication 86526/78 to Naganuma et 10 al (Lion Dentifrice Company) describes that liquid / solid separation in toothpastes with an anionic surfactant and a polyoxyethylene block copolymer type surfactant (ie, a "pluronic" surfactant) can be overcome by use of a binder or gelling agent of at least one substance selected from hydroxyethyl cellulose and / or xanthan gum, rather than carrageenan, tragacanth gum, sodium carboxymethyl cellulose, poly (sodium acrylate) or guar gum. The toothpastes described contain a surfactant such as gly-cerine, sorbitol, propylene glycol or polyethylene glycol.

The only surfactant mixtures described in specific formulations, including those that exhibit separation when a gelling agent other than hydroxyethyl cellulose or xanthan is used, contain glycerine and propylene glycol.

U.S. Patent 4,353,890 to Scott (Colgate-Palmolive Company) describes toothpastes containing carrageenan gelling agent stabilized by microwave radiation to maintain viscosity. A dicalcium phosphate toothpaste with such a stabilized carrageenan with a mixed humectant of 4.5 wt.% Glycerol and 17.5 wt.% Sorbitol is shown in the examples and is described by storage tests, including also in packages containing container portions 35 of polyethylene. The detergent or surfactant used in the examples is sodium lauryl sulfate. The patent includes a general description of "Pluronic®" as detergents.

It is an advantage of the present invention that phase separation of a toothpaste packaged in contact with a polyolefin material which would undergo phase separation if no additive inhibiting syneresis is present is substantially avoided. Other advantages will be apparent from the following description.

In accordance with a number of aspects thereof, this invention relates to a packaged toothpaste, wherein the toothpaste is in direct contact with a low or medium density polyethylene or polypropylene surface, in which syneresis takes place in said toothpaste because of the direct contact as the toothpaste substantially consists of -15 ingredients of 20-75 wt% liquid carrier consisting essentially of 10-50 wt% water, about 5.0-15 wt% glycerine and sorbitol, the amount of glycerine and sorbitol together about 15- 50 wt%, and a glycerin to sorbitol weight ratio of from about 0.25: 1 to about 1: 1, about 0.05-10 wt% of a toothpaste gelling agent selected from the group consisting of Irish Moss, gum tragacanth, sodium carboxymethyl cellulose, hydroxyethyl cellulose, polyvinylpyrrolidone, sodium alginate, guar gum, starch, xanthan and iota_carragenan and about 25-75% by weight of a dentally acceptable water-insoluble calcium or mag nesium alkaline earth metal salt polishing agent; wherein said toothpaste mainly consists of these ingredients and as the only additive to counteract syneresis in the toothpaste on direct contact, about 0.1-5 wt% of a nonionic polyoxyethylene-polyoxypropylene block copolymer.

In toothpaste formulations, the liquids and solids are necessarily in that ratio to form a creamy mass of the desired consistency extrudable from its package. The liquids in the present toothpaste mainly comprise water, glycerine and sorbitol. The total liquid carrier is about 20-75% by weight of the formulation.

A gelling agent in the toothpastes is a natural or synthetic gum or gum-like material, especially such as Irish moss (carrageenan), gum tragacanth, sodium carboxymethyl cellulose, hydroxyethyl cellulose, polyvinyl pyrrolidone, sodium alginate, guar gum, starch], xanthan or iota. carrageenan, and mixtures thereof. Irish moss, sodium carboxymethyl cellulose, and iota carrageenan, as well as mixture thereof, are particularly compatible and are the preferred gelling agents. The gum content is about 0.05-10% and preferably about 0.5-5% by weight of the formulation.

Water is included in toothpaste in an amount of about 10-50% by weight, preferably about 15-35%. Glycerin and sorbitol together generally comprise about 15-50% by weight, preferably about 20-35% of the toothpaste, with the amount of glycerine about 5.0-15% by weight and the weight ratio of glycerine 20 to sorbitol about 0.25: 1 to about 1: 1, typically from about 0.25: 1 to about 0.8: 1, and preferably from about 0.25: 1 to about 0.6: 1. It is preferred to use about 6-10 wt% glycerine and about 17-24 wt% sorbitol. Amounts of sorbitol 25 as used herein refer to sorbitol syrup as commercially available i.e.

70 wt% sorbitol in 30 wt% water.

A dental acceptable water-insoluble alkaline earth metal salt polishing agent is present in the dental paste in an amount of about 20-75% by weight, preferably about 35-60%. Typical salts include dicalcium phosphate dihydrate, anhydrous dicalcium phosphate, calcium carbonate, tricalcium phosphate, calcium pyrophosphate, dimagnesium phosphate trihydrate, and magnesium carbonate as well as mixtures thereof. More in particular, a calcium salt, preferably dicalcium phosphate dihydrate or a mixture of dicalcium phosphate dihydrate and anhydrous dicalcium phosphate, is present.

In addition to the alkaline earth metal salt polishing agent, additional polishing agents may be present. such as hydrated alumina and calcined alumina, for example, in a weight ratio of alkaline earth metal salt to alumina material from about 2.5: 1 to about 4: 1, the total amount of polishing agent in the toothpaste being about 25-75% by weight.

The only material used in the present invention to counteract syneresis when the toothpaste is in direct contact with a layer or medium density polyethylene or polypropylene is a nonionic polyoxy-15 ethylene-polyoxypropylene block copolymer. The block copolymer is also effective in the toothpaste as a surfactant. It is present in an amount of about 0.1-5% by weight, preferably about 0.5-3%.

The nonionic surfactant used in the present invention is a block copolymer containing polyoxyethylene and polyoxypropylene. Such block copolymers are available from Wyandotte Chemicals Corporation under the trade name "Pluronic". These can be liquid, pasty or solid and are generally chemically defined in terms of the molecular weight of the polyoxypropylene hydrophobic group and the weight percentage of the polyoxyethylene hydrophilic group. The following block copolymers are available from Wyandotte: c @ 8024 6 0 -8-

Pluronic Physical _ MW, _ number character Hydrophilic Hydrophobic L121 liquid 10 4000 LL01 liquid 10 3250 L 81 liquid 10 2250 L 61 liquid 10 1750 5 L 31 liquid 10 950 L122 liquid 20 4000 L 92 liquid 20 2750 L 72 liquid 20 2050 L 52 liquid 20 1750 10 L 42 liquid 20 1200 P 123 paste 30 4000 P 103 paste 30 3250 L 63 liquid 30 1750 L 43 liquid 30 1200 15 P 104 pasta 40 3250 P 94 paste 40 2750 P 84 paste 40 2250 P 64 liquid 40 1750 P 44 liquid 40 1200 20 P 105 paste 50 3250 τι n _ cr \ 2250 P 85 paste 50 dtc. or 2050 P 75 pasta dcc 4.5Ω 1750

P 65 pasta DU

qc η P 35 liquid 50 25 F 127 fixed 70 4000 F 87 fixed 70 2250 P 77 fixed 79 2050 F 108 fixed 80 3250 F 98 fixed 80 2750 30 F 88 fixed 80 2250 F 68 fixed 80 1750 F 38 fixed 80 950, S 8 G> 2 4 β 0 -9-

The preferred nonionic block copolymers are solid (or flake) materials and most preferred are Pluronic F-108 (80% polyoxyethylene: 3250 mw polyoxypropylene and F-87 (70% polyoxyethylene: 2250 mw polyoxypropylene), 5 F-127 (70 % polyoxyethylene: 4000 mw polyoxypropylene) and L-72 (20% polyoxyethylene: 2050 mw polyoxypropylene).

Since the nonionic block copolymer provides substantially no foam to the toothpaste, a nonionic surfactant may also be present due to its foaming character and to enhance cleaning performance. The surfactants may have increased prophylactic action, assist in achieving thorough and complete dispersion of the present composition through the oral cavity, and make the toothpastes more cosmetically acceptable.

Suitable anionic surfactants are the water-soluble salts of higher fatty acid monoglyceride monosulfates, such as the sodium sulfate of the monosulfated monoglyceride of hydrogenated coconut oil fatty acids, higher alkyl sulfates, such as sodium lauryl sulfate, olefin sulfonate, such as sodium dodecyl benzene Contains 22 carbon atoms, higher alkyl sulfoacetates, higher fatty acid esters of 1,2-dihydroxy-propane sulfonates and the substantially saturated higher aliphatic acylamides or lower aliphatic aminocarboxylic acid compounds such as those with 12-16 carbon atoms in the fatty acid, alkyl or acyl radicals and the like. Examples of the latter amides are N-lauryl sarcosine, and the sodium, potassium, and ethanolamine salts of N-lauroyl, N-myristoyl, or N-palmitoylsarcosine, which should be substantially free of soap or the like higher fatty acid material that tends to significantly diminish the effect of these compounds in compositions of the present invention. The amides are more particularly preferred, as they exhibit an elongated and <8802460-10- activity in inhibiting acid formation in the oral cavity due to carbohydrate breakdown in addition to exerting some reduction in the solubility of tandem enamel in acidic solutions. Another desired material is a long chain fatty acid sodium monoglyceride sulfonate alone or in combination with sodium lauryl sulfate. It is preferred to use about 0.2-5 wt% total surfactant, typically about 1-3% when anionic surfactant is present.

In general, the toothpaste may also contain a fluorine-containing compound having a beneficial effect on the care and hygiene of the oral cavity, such as reduction of enamel solubility in acid and the protection of the teeth against degradation. Examples thereof include sodium fluoride , tin fluoride, potassium fluoride, potassium tin fluoride (SnF2.KF), sodium hexafluorostanna, tin chlorofluoride, sodium fluorozirconate and sodium monofluorophosphate. These materials which dissociate or release fluorine-containing ions in water may be suitably present in an effective but non-toxic generally in the range of about 0.01-1% by weight of its water-soluble fluorine content.

The preferred fluorine-containing compound is sodium ananonofluorophosphate, typically present in an amount of about 0.076-7.6 wt%, preferably 0.76%.

A mixture of sodium monofluorophosphate and sodium fluoride is also advantageous, for example, in a weight ratio of about 2: 1 based on fluoride.

Any suitable flavor or sweetener may be used in formulating flavor for the composition of the present invention. Examples of suitable flavor components include the flavor oils, such as oils of spearmint, peppermint, wintergreen, sassafras, cloves, sage, eucalyptus, cinnamon, lemon and orange, as well as methyl salicylate. Suitable sweeteners include sucrose, lactose, maltose, xylitol, sodium 6-methyl-3,4-dihydro-α. 0 2.4 6 0 -11- 1,2,3-oxathiazine-4-one, sodium, cyclamate, perillartine and sodium saccharin. Generally, the flavors and sweeteners together may contain from about 0.01-5% or more of the compositions of the present invention.

Various other materials can be included in the toothpaste. Examples thereof are dyes or whiteners or paints, anti-decay agents such as sodium benzoate, anti-corrosion agents, silicones, chlorophile compounds, ammonia materials such as urea, diammonium phosphate and mixtures thereof and other components. Whitening agents, such as titanium dioxide, typically in amounts of about 0.5-2% may be beneficial to the appearance of the toothpaste composition, since some discoloration may occur with aging.

The additives are included in the present compositions in amounts which do not substantially adversely affect the desired properties and characteristics, and are selected and used in appropriate amounts depending on the desired composition.

Antibacterial agents can also be used in the oral compositions of the present invention in amounts of about 0.01-5% by weight. Typical antibacterial agents include: 1 N - (4-chlorobenzyl) -N - (2,4-dichlorobenzyl) biguanide; P-chlorophenyl biguanide; 4-chlorobenzhydryl biguanide; 4-chlorobenzhydrylguanylurea; N-3-lauroxypropyl-N-chlorobenzyl biguanide; 1.6-dichlorophenylbiguanidohexane; 1,6-bis- (2-ethylhexylbiguanido) hexane; 1- (lauryl dimethyl ammonium) -8- (p-chlorobenzyldimethyl ammonium) octane dichloride; 5.6-dichloro-2-guanidinobenzimidazole; N-p-chlorophenyl-N-lauryl biguanide; 5-amimo-1,3-bis (2-ethylhexyl) -5-methylhexahydropyrimidine and non-toxic acid addition salts thereof.

.8802460 -12-

Various calcium and magnesium ion suppressants can also be used to adjust the physical properties of the compositions. Suitable agents are the water-soluble inorganic polyphosphate salts, such as tetrasodium pyrophosphate or disodium pyrophosphate, with the partially neutralized or polyphosphate being preferred. Other suitable agents are the alkali metal, preferably sodium, citric acid salts. In general, such compounds 10 will represent a minor amount or ratio of the formulation. The exact amount will vary depending on the specific formulation, such as the physical characteristics of the toothpaste, but will generally range from about 0.1% to about 3% by weight.

Toothpastes should have a pH value suitable for application. A pH range of 5-10 is particularly desirable. The reference to pH refers to the pH determination directly on the toothpaste.

If desired, materials such as citric acid can be added to adjust the pH to, for example, 6 to 7.

The packaging in which the toothpaste is incorporated can be any polyolefin laminate toothpaste tube. For example, the tube may be as elemental as described in U.S. Patent 3,260,410 to Brandt et al, the disclosure of which is incorporated herein by reference. As indicated in the example thereof, an aluminum foil base with a thickness of about 0.0013 cm was heated to a temperature of about 177 ° C, 30 and a surface of the heated foil was contacted with an extrudable foil of a random- copolymer of ethylene and acrylic acid (acid content 3 + 0.5% and melt index 8 + 1), while the other surface thereof was applied against a film of low density polyethylene. Using powered rollers, a laminated base was obtained in which the copolymer layer 8802460 -13- was about 6 millimeters thick and the polyethylene layer was about 5 mils thick. The base was then formed into the correct tubular shape and welded.

After cutting the tube into the tube bodies, the tubes can be filled with the toothpaste of the present invention without the toothpaste undergoing syneresis.

Polyolefin laminate multi-layer toothpaste tubes can also be successfully used in conjunction with the toothpaste of the present invention without undergoing syneresis. For example, the multilayer flexible layer structure for toothpaste tubes described as prior art in Eckstein's U.S. Patent 4,418,841 can be used as can the more tear-resistant structures also described therein. The description of Eckstein's U.S. Patent 4,418,841 is herein included for reference. Indeed, toothpastes of the present invention packaged in layer material tubes identified as Prior Art A 20 and A-1 in U.S. Patent 4,418,841 are particularly satisfactory and substantially do not undergo syneresis. Such tubes A and A-1 are made up of layers as indicated below in the order from the outer layer to the inner layer.

25 A_ A-1

1.5 mil LDPE 1.5 mil LDPE

2.0 mil pigmented LDPE 2.0 mil pigmented LDPE

1.6 mil paper 1.6 mil paper

0.7 mil LDPE 2.0 mil LDPE

30 3.3 mil EAA 1.0 mil OPP

0.7 mil foil 1.0 mil EAA

2.0 mil EAA 0.7 mil foil

1.2 mil LDPE 2.0 mil EAA

13.0 mil total 1.2 mil LDPE

13.0 mil total. 8802 460 -14-

In A and A-1, the abbreviations have the following meanings: LDPE low density polyethylene EAA ethylene acrylic acid OPP oriented polypropylene 5 Middle density polyethylene can replace low density polyethylene. In toothpaste "sachets" packaging, medium density polyethylene is preferred.

Mechanically operated dispensers, such as the dispenser for, in particular, paste-like substances, described in U.S. Patent No. 10,4437,591, to von Schuckmann, the disclosure of which is incorporated herein by reference, may also be used in the embodiment. of the present invention. The housing of such devices generally consists of a polyolefin resin such as polypropylene.

Therefore, the resin of the housing is essentially a layer, the inner surface of which is in contact with toothpaste. When the toothpaste of the present invention is packaged in such a polypropylene mechanical dispenser, it essentially does not undergo syneresis.

The following properties are typical therein for low and medium density polyethylene 8802460 -15-

Brightness LDPE_MDPE__ transparent transparent up to _translucent translucent_ 30,000 29,500 in2 / lb / 0.001-in "yield" 1,085,000 1,065,000 cm2 / kg / 0.0Qi-cm)

Specific 0.910-0.925 0.926 Density 0.940 5 Tensile Strength 1,000-3,500 2,000-4,000 lb / in2 ASTM D-882 (6,900-24,150 13,800-34,500 kPa)

Elongation (%) 225 - 225 - ASTM D-882 600 500

Impact resistance 10 (kg-cm) 7-11 4-6

Tear strength 100-400 50-300 g / 0.001 in Eïtiendorf ASTM D-1922 (250-1.000) 125-750 g / 0.001 cm (lmendorf)

Heat weldable - 250-350 260-310 ° F

range (120-175 125-155 ° C

15 WVTR 1.2 0.5-1.0 g / 24hr / 100 in2. 100 ° F

90% RH (7.74 3.23-6.45 g / 24hr / 100 cm2

ASTM E-96 '37 ° C

, 3862460 -16-

LDPE MDPE

Gas Flow - 250-840 165-335 cc / 0.001-in. / LOOin2 /

^ 24 hr. ATM 73 ° F + 0% RH

2 0 -ASTM D-1434 (150-515 100-205 cc / 0.060 cm / 100 cc / 2 24 hr ATM22.77 ° C + 0% RH) 5 495-5.000 500-840 cc / 0.001-in / 100in2 /

24 hr. ATM 73 ° + 0% RH

Gas permeability CO-ASTM (300-3,050 305-515 cc / 0.001 cm / 100 cm / D-1434 24 hr A ™ 22.77 ° C + __0% RH)

Resistance to grease and oil _varies_good_-

Maximum usage. 150 180-220 at lü temperature (0 C) (65.5 82-105 o ^

Minimum use -60 -60 ° F

temperature (-C) (-51 -51

Dimensional none

change at high RH

(%) __ ^ 5 Machine behavior fairly reasonable

Printability good after treatment after treatment division

Heat shrinkable certain types certain types

Typical of polypropylene types that can be used particularly as a toothpaste dispenser housing are those supplied by Shell Chemical Company as polypropylene DP 5A03 and polypropylene DP 5A03S. These controlled rheology products combine the processability of melt flow index 12 types with higher impact strength in practice (as measured by falling weight test).

t 8802 460 -17-

These types are designed for fast processing in molds with many cavities.

Polypropylene types DP 5A03 and DP 5A03S have the following general properties:

^ Tradition- SI A-ASTM

single units test _units_

Melt flow 12 g / 10 min 12g / 10 min D 1238 ^

Density 23 ° C 0.905 g / cc 0.905 g / cc D 1505 10 "Tensile yield strength" 2 at 5.0 cm / min. 5000 psi 34 MPA D 638 "Yield elongation" at 5.0 cm / min. 9% 9% D 6382 1% Secant modulus, 15 at 0.5 cm / min 190,000 psi 1300 MPa D 6382

Flexural modulus, at 0.13 cm / min, 200,000 psi 1375 MPA D 790A2 5 cm span

Izod Notched Impact Resistance Λ 20 at 73 ° F / 23 ° C 0.5ft-lb / in 26 J / m D 256 Λ at 0 ° F / -18 ° C 0.3 ft-lb / in 15 J / m D 256

Hardness Rockwell R92 R92 - D 785 HDT at 66 psi / 455 kPA 220 ° F 104 ° C D 648

Vicat softening temp. 305 ° F 152 ° C D 1525 25 ^ Condition 230 / 2.16 2 ASTM type I sample, 0.32 cm thickness (injection molded sample)

The advantages of the present invention are also present when the toothpaste is packaged in a flexible package with a polyolefin surface, generally of low density or medium density polyethylene.

The following illustrative examples serve to further illustrate the nature of the present invention, but it will be understood that the invention is not limited thereto. All amounts and ratios are by weight unless otherwise indicated.

. $ 862460-18-

EXAMPLE I

The following toothpastes are prepared to creamy consistency and packaged in tubes of each of the laminated structures A and A-1 as described above.

5 Share

A B

Glycerin (99.3%) 10.00 10.00

Sorbitol (70%) 17.00 17.00

Na carboxymethyl cellulose 0.95 0.95 Na saccharin 0.20 0.20

Tetrasodium pyrophosphate 0.25 0.25

Na monofluorophosphate 0.76 0.76

Dicalcium phosphate dihydrate 48.76 48.76 _

Na lauryl sulfate 1.10 1.10 15 Flavor 0.89 0.89

Pluronic F-108 0.50

Water Q.S. to Q.S. up to 100.00 100.00

After aging for 8-10 days at room temperature, toothpaste B begins to undergo syneresis and phase separation. Toothpaste A remains stable against such phase separation after aging at room temperature for periods of more than 1 year.

EXAMPLE II

Toothpastes A and B are contained in a mechanical dispenser according to US Patent 4,437,591, which consists of a polypropylene housing. Toothpaste A retains its creamy consistency, while toothpaste B separates into liquid and solid phases.

Similar results to those described above are obtained as: 1) Pluronic F-127 and F-87 replace F-108; 2) Pluronic L-72 replaces Pluronic F-108; 3) Pluronic F-84 replaces Pluronic F-108; 4) the comparative amounts of glycerine and sorbitol (70%) are: 5:20 and 12:15; .Ö & 02460

a

-19- 5) Irish moss and iota carrageenan replace sodium carboxymethyl cellulose; 6) the toothpastes are packaged in laminated tubes according to U.S. Patent No. 5,260,410; 7) the toothpastes are packaged in tear-resistant laminated tubes in accordance with U.S. Patent 4,418,841; 8) the toothpastes are packed in flexible sachets of the following structure from the outside in; 12.2 yum polyethylene terephthalate 21.3 ^ im white ethylene acrylic acid 9.0 yum foil ..

3.3 µm ethylene acrylic acid 25.4 µm MDPE; and 9) a mixture of 0.3 parts of sodium carboxymethyl cellulose and 0.6 parts of iota carrageenan replaces the sodium carboxymethyl cellulose as the sole gelling agent.

Obviously, the foregoing detailed description is given by way of illustration only, and variations may be made there without departing from the spirit of the invention.

* 8102460

Claims (10)

1. Packaged toothpaste, wherein said toothpaste is in direct contact with a low or medium density polyethylene or polypropylene surface, in which syneresis occurs in the toothpaste because of the direct contact when the toothpaste mainly consists of ingredients 20-75% by weight of a liquid carrier consisting essentially of about 10-50 wt% water, about 5-15 wt% glycerine and sorbitol, the amount of glycerine and sorbitol together being about 15-50 wt%, and wherein the weight ratio of glycerin to sorbitol is from about 0.25: 1 to about 1: 1, about 0.05-10 wt% of a toothpaste gelling agent selected from the group consisting of Irish moss, gum tragacanth, sodium carboxymethyl cellulose, hydroxyethyl cellulose, polyvinylpyrrolidone, 15 sodium alginate, guar gum, starch, xanthan and iota-carragenan, and about 20-75% by weight of a dentally acceptable water-insoluble calcium or magnesium alkaline earth metal salt polishing agent; which toothpaste mainly consists of said ingredients and as the sole additive for combating syneresis in the toothpaste contains, in said direct contact, about 0.1-5% by weight of a non-ionic polyoxyethylene-polyoxypropylene block copolymer. The packaged toothpaste according to claim 1, wherein the weight ratio of glycerine to sorbitol is from about 0.25: 1 to about 0.8: 1. The packaged toothpaste according to claim 1, wherein the block copolymer is a solid material. The packaged toothpaste according to claim 3, wherein the solid block copolymer contains about 80% by weight hydrophilic polyoxyethylene content and has a hydrophobic polyoxypropylene molecular weight of about 3250. The packaged toothpaste according to claim 1, wherein the gelling agent is sodium carboxymethyl cellulose, in an amount of about 0.5-5 wt%. c S8 02.4 6 0 -21- * The packaged toothpaste according to claim 1, wherein the water-insoluble alkaline earth metal salt is a calcium salt. The toothpaste according to claim 6, wherein the calcium salt is dicalcium phosphate dihydrate. The packaged toothpaste according to claim 1, wherein the toothpaste is packaged in a plastic laminate tube, wherein the inner surface consists of low density polyethylene. The packaged toothpaste according to claim 1, wherein the toothpaste is packaged in a mechanical dispenser with a polypropylene resin housing. The packaged toothpaste according to claim 1, wherein the toothpaste is packaged in a flexible sachet, the inner surface of which is low-density polyethylene or medium-density polyethylene. .8 * 02 450