Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.
~2~2
,
., .
., ,
The present invention relates to on anti plaque dentin
rice containing a ~uaternary active ingredient and at least
1.5~ and up to I button surfactant by weight, such as cocos :
amidopropylbetaine~ lauramidopropylbetaine, cocobetaine t etc.,
which enhances foaming and does not inactivate the antibacterial
activity of the qua ternary compound. Non ionic surfactants fair
to afford sufficient foaming, and anionic sur~actants inactivate
the qua ternary antibacterial activity Carbowaxi~600 (posy-
elan glycol) and/or sorbitol replace propylene glycol and
glycerin a humectant~ in order to afford stability to the
betaine-containing composition. Also carboxymethyl cellulose
is pre~erably;avoided because large organic~molecules~deactivate Jo
the qua~ernar~compound~. Non ionic gums such as hydroxyethylcell~
Ulysses used as gelling/~hickening agent for eke dental cream.
More:specirically~ this composition issuer Or anionic and Jo
non~onic surfactants and~con~ains only a minimal amount of
glycerin, 1~10%`and~preferably 5-7~ by weight as fluoride ::
stabilizer (when a fluoride compound is used) in 8 sole~poly
ethylene glycol humectant-oontaining composition.
Jo 7 /2 A/ D A
:: :: : : :
-2-
If i
i!
I
If ,
i- :
I ,
Jo It has been ode that the addition of a button
~ur~actant to an anti plaque dental formulation based on utter-
nary active ingredients, improves the foaming characteristics
, thereof, without deactivating the qua ternary antimicrobial
, astute It has additionally been found what humectants other
than glycerin are required on the button system to effect
i
cosmetic stability,, specifically polyethylerle glycol and/or
sourball The limitation ox the gelling/thickening agent to
anionic gums such as hydroxyethylcellulose is also a necessary
expedlent9
The ability of qua ternary ammonium compounds Jo inhibit
the formation of dental plaque is well documented. These coy
pounds, however present a problem when formulated in a dentin
rice in that they are deactivated by traditional anionic
surfac~ants such as sodium laurel sulfate. Stable, clinically
effect dental formulations have been made with qua ternary
; I: ammonium compound sand non ionic surfactantsg but these formula-
lions arriver poor framers and result in inferior products.
Compositions containing anti plaque qua ternary ammonium compounds
~and:nonionic surfactant6 are disclosed in U. S. Patent6~No.
4,0~0,~41, No. Noah. 4,11g,472, No. 4,11~7473, No.
I; I` I 475~ No 4,11~,476, and British Patent No. 1,573,356
: : : :
:
--3
I
i
l,
If 2 3 8 Z
11
i
Al
:
Us S. Patent No. 4,161,51~ discloses a dentifrice
¦¦ composition or inhibiting plaque formation containing 0.05~
I by weight of a qua ternary ammonium organosiloxane as the active
it antibacterial agent in a suitable vehicle co~tai~i~g suitable
polishing agents, fluoride compounds 9 anionic surfactants,
flavoring and sweetening agents, thickening agents such as
: carboxymethylcellulose 9 humectants such as glycerin, sorbitol
and other polyhydric alcohols.
U. S. Patent No. 3,9B~,435 discloses pharmaceutical
compositions including a dentifrice containing a quatrain
ammonium dihydrochalcone glucoside as the antibacterial agent
having a sweet waste, US well as abrasives, surfactants including
nonionics and "derivatives of fatty amine with button struck-
Ursula swelling, guying or thickening agents such as hydroxy-
alkylce}lul~se particularly hydroxyethylcellulose, polyethylene
glycols, polypropylene glycols, etc., humectants such as sorbitol,~
I minutely, glycerin propylene glycoI~ colorants, and flavors.:
:
: All of aforesaid cited patents simply list the con-
: : ventional additi~es:useful in dentifrice compositions There
is no disclosure ox the use of the button as the exclusive
;surfactant in the production of a high roaming dentifrice, There
:1
,: :
:
-4- ;
If i
I 32
., t
1, :
"
¦¦ is also no disclosure nor recognition of the necessity to limit
Jo the humectaAt Jo polyethylene glycol and/or -orbital and the
II thickening agent to anionic gums such a hydroxyet~ylce~lulose 7
in order to obtain a cosmetically stable dentifrice in a button-
quit system.
i U. S. Puissant No. ~,363,795 and its counterpart
i International Patent Publication No. We ~0/000~7 to Wahlstam
; disclose a cleaning agent for destine surfaces containing a
qua ternary minim oompound9 an ampholytic tinseled which may be
an imldazoline or a button and a sequestering agent of the
~mtinocarboxylic acrid type which has a synergistic effect as to
the antibacterial properties of the treating solution. All the
:
examples are in the form of cleaning solutions There is no
I: I mention of dental reams, nor the use of~humectants and thicken- :
in agent
Us So Patent No 4,130,637 discloses a specific group
I of b~taine compounds, or a mixture of said button and its
:
. corresponding carboxylic acid qua~ernary ammonlum salt in a
9:1 ratio, as non~staln~ng antimicrobial anti plaque agents in
a dent1frice~ehicle containing the aforelisted conventional
: : i
t' : :
:
5- :
lZ~38Z8~
If ,.,
I' i
¦ humectan~s and golfing agents, and a non ionic sur~actant~ This
patent fails to disclose the necessity of using a button sun-
vacant exclusively, the specific non ionic golfing agent
ii hydroxyethylcellulose and the specific humectant polyethylene
glycol and/or sorbitol, in order to obtain a stable, high foam-
in quat~rnary-containing anti plaque dentifrice.
! u. so Patent Nos. 4,117,107 and 4,117910~ also disclose
a specific group of button compounds and their salts as anti-
plaque agents in a dentifrice vehicle containing the conventional
humectants and galling agents, as well as anioniG/nonionic sun-
: fact ants There is no disclosure ox an antibacterial qua ternary
: smmonium compound, and a button surfactan~ exclusively. There
is also no recognition of the specificity of humectant and
golfing agent and the exclusion of anionic/nonionic surfactants
:
: in ~:quaternary-betaine system, which is necessary in order to
obtain a enable high foaming anti plaque dentifrice
However, none of the above cited prior art discloses
: : cosmetically stable anti plaque dentifrice with improved foam-
in and fluoride stability containing as the essential ingredi- :
: ,` eights cat ionic qua ternary ammonium anti plaque compound a :
I' zwitterionic button sur~actant, humectant compatible with
: .. :
`
:
-6
it
¦ the cat ionic anti plaque agent selected from the group consisting
¦¦ of polyethylene glycol and sorbitol, and the non ionic golfing
agent hydroxyethylcellulose~ in an aqueous vehicle containing
a dental abrasive Nor is there a prior art disclosure of the
sourball humectant improving long term fluoride stability, nor
; the combination of small amounts of glycerin in a polyethylene
glycol humectant improving long term fluoride stability.
.
Summary of the Invention
: It has now been found that dental cream formulations
containing anti plaque qua ternary ammonium compounds may be
stabilized and provide better foaming when button type surface-
ants replace the traditional anionic and non ionic surfactants.
: : Humectants such as polyethylene glycol and sorbitol must replace
the conventional glycerin for better cosmetic stability of the
: product. However, a small amount of glycerin may be used to
: chemically stabilize the fluoride-containing compound in a sole
polyethylene glycol humectant. Non ionic gums such as hydroxy-
ethyl cellulose replace the anionic carboxymethylcellulose golfing
: 1 agent which also has the potential to deactivate the ~uaternary
jl~ompound~ :
-7-
- !! i
If
Jo
., .
~L~3~3~82
,1
l i
Accordingly, a primary object of the preset invention
is to provide a better foaming anti plaque dentifrice based on
l! qua ternary assay ingredients by the incorporation of a whetter-
'ionic button surfactant as the foaming agent.
.. Another object of the present invention is to provide I
a cosmetically stable foaming anti plaque dentifrice containing
polyethylene glycol and/or sorbitol as hum~ctan~ which is come
partible with the byway and the qua ternary active ingredients.
i . Still another object of this invention is to provide
actable foaming antlpIaque dentifrice containing thy non ionic
:
gum, hydroxyethyl:cellulose, as golfing agent to stabilize the
betaine-~uat system and to prevent deactivation of the qua ternary
active lngredient~by the anionic sites on molecules Or car boxy-
ethyl cellulose
nether object of this invention is to provide a :
cosmetic (physical and chemically stable foaming anti plaque
den~ifrice~contai~ing a fluoride-providing compound andlsorbitol
or minimal~amounts:of glycerin, Lyle by weight as;seabilizlng
agents o'er tho~fluoride-providing compound",~without~adverse1y
affecting cosmetic stability ox the dentifrice. I :
j
: : ,
I
Jo C
:: : :
32
I
" .
. '.
¦ Additional objects, advantages and novel features
of the invention will be set forth in part in the description
which follows, and in part will become apparent Jo those skilled
in the art upon examination of the following or Jay be learned
i by practice of the invention. The objects and advantages of
i the invention may be realized and attained by means ox the
instrumentalities and combinations particularly pointed out in
the appended claims.
To achieve the foregoing and other objects and in
accordance with the present invention, as embodied and broadly
: described herein, the novel stable foaming anti plaque dentifrice
Or this invention comprises as thy essential ingredients, a ; :
: : : :
qua ternary ammonium anti plaque compound, a zwitterionic button : ;
surfactan~ a humectant selected from the group consisting of
polyethylene glrcol~ sorb~tol and mixtures thereof,~a~nonionic
; gelline~agent; swishes hydroxyethylcellulose and preferably a
Jo fluoride-provlding;compound, in an aqueous vehicle containing
,
a dental abrasive.
: More specifically, present invention relates to a
:;~ stable anti plaque dentifrice formulation with improved foaming :
and fluoride sublet comprising an effective antimicrobial
I
:: :
I
amount of a ~uaternary ammonium compound, about 1.5-2% by
weight button, about 20-30% by weight humectant selected from
the group consisting of polyethylene glycol, sorbitol and mix-
lures thereof, about 0.5-2% hydroxyethylcellulose, and about
0.05-2% by weight of a fluoride-providing compound, in an
aqueous vehicle containing about 40-60% water insoluble dental
abrasive. The sorbitol component, which stabilizes the
betaine-quat system, also improves long term fluoride chemical
stability of the dentifrice. In a sole polyethylene glycol
humectant, a small amount of glycerin, as low as 1%, may be
utilized to improve long term fluoride stability, without ad-
tersely affecting the cosmetic stability ox the dentifrice.
Cat ionic antibacterial materials are well known in
the art. See, for instance the section on "Qua ternary Ammonium
and Related Compounds" in the article on "Antiseptics and Disk
infect ants" in Kirk-Othmer Encyclopedia of Chemical Technology,
end edition (Vol. 2, pp. 632-635). Cat ionic materials which
possess antibacterial activity (i.e. are germicides) are used
against bacteria and have been used in oral compositions to
counter plaque formation caused by bacteria in the oral
cavity .
-- 10 --
l, i
J
38Z8;~
!
I'
! i
Among the most common of these antibacterial anti plaque
qua ternary a~moniwm compounds is benzethonium chloride, also
known as Hymen 16~2 or diisobutylphenoxyethoxyethrl dim ethyl
bouncily ammonium chloride, and Seattle pyridinium chloride In an
oral preparation this material is highly effective in promoting
tonal hygiene by reducing formation Or dental plaque and calculus,
wish is generally accompanied by a reduction in periodontal
diseases Other cat ionic antibacterial agents of this type are
those mentioned for instance, in U. S. Patent Nos. 2,9~4,639,
: 3,325,402, 3,~31,20~ and 3,703,5g3, and British Patent No. 1:,
~319,3~6.
: Other antibacterial anti plaque qua ternary ammonium
compounds include those in which one or two of the substituents
: on the quaternary:nitrogen has a carbonation length (typically
alkyd group) of Siam to 20, typically lo to lo, carbon atoms: :
while the remaining~substituents have a lower number of carbon :
atoms (typically~alkyl or bouncily group),~such~as l~to~7~carbon~ :
atoms, typically methyl or ethyl groups. Dodecyl trim ethyl I;
; ammonium bromide, benzyl~dimethyl stroll ammonium chloride,-;;
icetyl pyridinlum chloride and quaternlzed 5-amino-l~3-bis~(2~
: ¦ ethylhexyl~ -5-methyl~hexa:hydro-pyrimidine are typical;quaternary
i ammonlum antibac~erisl agents.
The de~tifrice:rormulation of present invention contains
an effective amount of the~antiplaque qua ternary ammonium come
pound, preferably about~O.Ol-5~9 and most preferably 00025-l~
by weight of the composition
:: :
.
ii ,,
1.23~
.
The ability of qua ternary ammon~um compounds to inhibit
the formation of dental plaque is well known. However, they
are deactivated by the anionic surfactants such as sodium laurel
sulfate conventionally used in dentifrice formulations. The
subs~itukion of non ionic surfac~ants for the anionic surfactants
eliminates the deactivation problem but results in products
with poor foaming :
The incorporation of button surfactants into antiplaqu~
dental formulations based on qua ternary active ingredients
unexpectedly improves the foaming of these formulations without
.
: de activating the qua ternary antibacterial agents.
: The button component of present dentifrice composition
has the general formula: :
R2 :
Rl-N~-R4-C00
R -
: : 3
:
wherein I is an alkyd group hazing 10 to about 20 carbon atoms
: prererably:12 to 16 carbon atoms or the~amido radical:
O H
: R-C-N-(CH2) _
I: : ! : :: a
,, : :
-12-
it !
,. ..
I
I!
,
whereon R is an alkyd group having about 10 to ZOO carbon atoms
I and a is the integer 1 to 3; R2 and R3 are each alkyd groups
hulling 1 to 3 carbons and preferably 1 carbon, R4 is an alkaline
or hydroxyalkylene group having from 1 to 4 carbon atoms and,
optionally, one hydroxyl group. Typical alkyldimethyl Betsy
. include decal b~taine or 2-(N-decyl-N,~-d~methylammonio) acetate,
.
coo button or 2-~N-coco-N,N-dimethylammonio) acetate, myristyl
button, palmltyl bstaine, laurel button, Seattle button, stroll
button, etc. The amidobetaines similarly include cocoamido-
ethyl button, cocoamidopropyl button, lauramidopropyl button
and the like.
Jo The battalions, which are zwitterionic materials,
function as a foaming agent in the quaternary-containing dentin
rice compositions. They act cationically over a wide fringe,
but do not deactivate the qua ternary antimicrobial activity. Jo
This is shinbone vitro tests using wool swatches:, which
Smalley human ski Nan oral tissue, as the absorptive material
in the Red::~O:Stain;test, J. Sock Comet, them. I 271-27~
(Swept",, Oust Lowe Wool has the same type of absorptive proper-
ties as oral tissue due to similar isoelectric and Seneca
,
I: : : ::
-13-
If, I
3~2~;~
I
I!
!
¦ points.
¦ Using the Red I Dye Test, the following experiment
illustrates thaw the button surfactan~ doesn't deactivate the
qua ternary. The Red I Stain Test was performed using a soul-
: lion of cocoamidopropyl button alone, benze~honium chloride
alone, and a mixture of cocoamidopropylbetaine and benzethoniu~
I chloride. The degree of staining of the wool watches treated
; with~benzethonium chloride alone and the mixture of benzethoniu~chloride and button was nearly equal, and both were stained
I : darker Han the cocoamidopropyl button treated swatch. This
induce chat benzethonium chloride is a "stronger" cat ionic
compound than the button i.e. it has a greater attraction to
he wool than the~betaine, indicating that the betaine~:doesn't
: deacti~ate~t:he ben~ethonium chloride
However, viol swatches treated with admixture of
benzethonium chloride and the anionic surfactant, sodium laurel
sulfate, exhibits no staining (no ridiculer retention) indict
ting~compleee:deactivation of the benzethonium~chloride by the
anionic surfac~ant.
The~deKree~of staining of the wool swatches trotted
;:
'I 1.
sly:
!;
¦ with a mixture of benzethon~um chloride and the non ionic sun-
¦ fact ant polyoxyethylene (20 moles ethylene oxide) sorbitan
: ! dyes turret, was substantially equal to that of the buoyancy-
thorium chloride alone. This indicates what the benzethonium
; chloride is not deactivated by the non ionic surfaotant.
In addition to the non-interference exhibited by the
: : " buttons with the qua ternary activity, laboratory foam tests
have shown that formulations containing both the quit and the
; button, roam 2-3 limes better than the nonionic/quat formula-
lions. The foam index for nonionic/quat compositions is about
,
20~ whereas the roam index for betaine/quat compositions is
about 40~60. The foam test used herein comprises placing I gram
of~the:test dentifrice in 10 ml of PPM water at 90F lea Jo
loo ml:graduated cylinder shaking furls seconds and riddling:
the foam height.
The zwitterionic buttons are completely compatible
with the~quaternary antimicrobial anti plaque agent sand impart
detersive and;improved~foaming properties to the qua ternary
containing d~n~ifrice~composition without deactivating the anti Jo
microbial properties thereof. The amount o~betaine elective :
: :: : :: :
: : :
-1 I
: :
I, ~2~8Z~32
Jo in the production of improved foaming may be varied from about
II 1D5-2~ active ingredient by weight of the total formulation.
'. Greater amounts of button adversely affect the taste of the
! .
dentifrice.
Cosmetic problems of stability is incurred with all
zwitterionic-containing dentifrices, such as crimp leakage
of flavor. The flavor oozes and is not soluO1lized in the
I; zwitterionic surfactant.
Accordingly, in order to effect cosmetic (physical)
lability of the button system, a specific group of:humectants
which includes polyethylene glycol, sorbitol or mixtures:thereor
must be used Glycerin and propylene glycol alone provide
: ins~fficient:cosmétic:stability to the button system. The
humectant system constitutes about owe Betty and preferably Jo
kiwi Andes selected prom the group consisting of polyethylene ;
glyco1~ sorbitol;and;mixtur s thereof.
Another essential ingredient in present dentifrice
is~a:gelling agent is a non ionic gum, in an amount up to: I;
5~by~weight;~:and:prererably about 0.5-2~. It~has~:been:round~
that:~large:organic anionic molecules~such~:as:carboxymethy~lce;llu~
lose Hiawatha potential to deactivate the qua ternary antibacterial
:
I:
: : ::
i
"
,,
11l ,,
¦¦ astute Ac~ordinglrl hydroxyethylcellulose, which is a non-
¦¦ ionic small organic molecule, effects a stable potatoes gel
¦¦ in the betaine-quat system of present invention, and is the
! preferred golfing agent. Other non ionic golfing agents may
be used such as hydroxymethylcellulose9 and the like.
It has been found that only by utilizing the specific
combination of ingredients of button, polyethylene glycol and/or
I sorbitol humectant and non ionic golfing agent, can a stable
anti plaque dentifrice with improved foaming based on the quoter-
nary antibacterial compounds, be obtained.
The fluoride-providing compounds, which ore preferably
I : : additional ingredients in present dentifrice, are characterized
:by~theirlability Jo release fluoride ions in water and by sub-
stantial:freedom from reaction with other compounds Or the
dentifrice. Among these materials are inorganic fluoride salts,
swishes soluble alkali metal, alkaline earth metal and heavy
metal~salts~;for example sodium fluoride, potassium fluoride,
:ammoniu~fluoride,~lead fluoride, a copper fluoride swishes
: cuprous M uoride, inferred, a tin fluoride swishes stunk
fluoride so swoons chlorofluoride, barium fluoride, sodium
fluorosilicate, ammonium flucrosilicate~ sodium~fluoro~.lrconate, Jo
dummy moncfIuorophosphate, aluminum moo- and di-fluorophosphate,
::
: : : : : : ; : : :
-17-
If i
I
i!
I ! ',
!,
and fluorinated sodium calcium pyrophosphate~ alkali metal
l! and tin fluorides, such as sodium and stuns fluorides, sodium
I monofluorophospha~2 and mixtures thereof, are preferred.
, The amount of the fluoride-providing keypad is
dependent to some extent, upon the type of compound, its oily-
blowout, and the dentifrice, but it must be a nontoxic amount.
In a solid oral preparation, such as a toothpaste or dental
cream an amount of such compound which releases a maximum of
1% by weight of the preparation is considered satisfactory
Any suitable minimum amount of such compound may be used but
it is preferable to employ sufficient compound to release from
O.OOSqO to I and preferably about Oily of;~Muoride ion. Typic
:
gaily, in the cases ox alkali metal fluorides and stuns
fluoride, this component is present in an amount up to 2% by :
White based on eta of the preparation, and preferably
Jo in the range of from 0.0~0 to Lowe In the case of odium moo-
:
~fluorophosphatev the compound may be present in an amount up
Tao kiwi by weigh, more typically owe
It has additionally been found that the long term
chemical fluoride stability in a sorbitol eased mectant or
a mixed sur~actant system containing polyethylene glycol and
:
:
:: :
If
,
ii
,
`
it 1;~38;~8~
i I
.
' ' '.,
at least I ,~,orbi~ol is markedly improved over a polyethylene
glycol based humectan~, whereon its fluoride stability is margin
at but acceptable However, the use of small amounts of glycerin
about 1~10% and pr~erably I by weight in a polyethylene
glycol based humec~an~ markedly improved long term fluoride
stability without adversely affecting the cosmetic stability
of present dentifrice formulation. The glycerin component herein
functions as, and is used as a chemical stabilizer for the
fluoride ingredient only when polyethylene~glycol is used as
the eye humectantO
Based on the three week results of the l20F aging study,
I glycerin improves the fluoride stability 25% without adversely
affecting cosmetic Sybil. The mechanistic reason why the
presence ox some glycerin improves the fluoride stability is
unclear. fluoride stability data after 12 weeks a loaf further
confirms the signl~icant improvement with the use ox small amounts
of glycerin in the dentifrice Table Clearly shows this imp
proved fluoride stability in a polyethylene glycol humeotant
:
system
: :
'.
I :
: !
:
:
:
--19--
II !
If
if
II ~L2382~
TABLE I
i Soluble Fluoride
' Glycerine:
i Polyethylene 3 woks 6 woks 9 woks 12 Waco
00 100 100 100
:20 0.093 0~077 owe 0.063 0.057
1:19 0.0~ 0.0~1 0.074 owe owe
: : 3:17 0.093 0.0~2 0.074 0.069 0.067
5 15 00093 Owe 0.077 0.071 0.070
I: Lucille : owe 0.0~3 owe 0.077
I: I : It has also been found that increase in the glycerin
content results in decreases in pi as shown in Table II.
BYE II : :
pi
~C pllv-tbyl~ 9 us
0:20 ; : I
., :
1:19 : 9,7 :
: ~3:17 : 9.4
: 5:15 :: 9~4
~0:10 .9 ::
: : : ; : :: :
:
-20-
I 1
1! 2 3 I 82
Jo
I .
if i
I The dentifrice of this in~ent~on, which it a toothpaste
10r dental cream, contains conventional water-insoluble polishing
aerials or dental abrasives, in amounts prom about 20-75% and
preferably about okay% by weight of the total formulation- Suit
able examples of dental abrasives or polishing materials include
: ' sodium metaphosphate, potassium metaphosphate9 tricalcium pros- .
photos dehydrated calcium phosphate an hydrous dicalcium phosphate,
calcium pyrophosphate9 magnesium orthophosphate, trimagnesium
phosphate, calcium carbonate alumina, hydrated alumina, aluminum
silicate, zirconium silicates, silica, bentonite, and mixtures
thereof.
Jo The dentifrice of this invention may also contain con-
; Yentional additional ingredients such us coloring or whitening
agents, preservatives, flavoring or sweetening materials, and Jo
: amounted materials such as monoammonium~glycyrrhizinate~ These
: additional ingredients may each be added Jo the dentifrice in
minimal amounts ox up to so by weight and preferably up to I -
provided they do not interfere with the foaming, anti plaque and
stability properties of the finished product
The dentifrice ox this invention is prepared by convent I :
: tonal methods Or making toothpaste and/or::dental~creams. More
I; I specifically a toothpaste may be prepared by:~forming~a gel with ;,hydroxyethylcellulose~and water adding~th2reto~with~ixing the
powdered materials including the fluoride compound and humectant,
: followed by the addition with mixing of polishing agent and then
: the button and favor and tubing the final mixture.
Jo
:
-21-
3~32~
In the practice of this invention to promote oral
hygiene, the dentifrice according to this invention is applied
regularly to dental enamel by Bryan the teeth or 30-90
seconds at least once daily.
.
Detailed Description of to Invention
The following examples are further illustrative of the
nature of the present invention, but it is understood that, two
invention is not limited thereto. The compositions are wrapper
in the usual manner and all amounts and proportions ref~rrcd
to heroin and in the appended claims are by weight unnails ox or-
wise indicated.
Aureole
` Hydroxyethylcellulose .0
Carbowax~600~ 20.0
No Saccharin 0.2 Jo
MFp2~ owe ;
GOB owe ; 3~5
Dicalcium~Phosphate 9.0
B~C}4 0.5
Do H20
Louvre 1.0
Polyethylene glycol,~ mol. weight 60
Sodium monofluorophosphate
3Cocoamidopropyl button
~Ben~ethonium chloride
I: : : : :
-22- :
32~%
:1
"
The hydroxyethylcellulose and water are premixed for
10 minutes to form a gel. The powdered materials MOP, clue
¦ and saccharin, and the Carbowax humectant is added to the gel
it and mixed for 10 to 20 minutes. The golfed mixture is added
,! to dicalcium phosphate and mixed for 20 minutes a speed in
the Ross agitator. The button and flavor is added to the mixture
' and mixed or 5 minutes at speed 6 in the Ross agitator. The
)'! resultant dental cream which is cosmetically attractive is
:
, tubed.
Aging tests performed on this product in lined tubes
at room temperature, 40 F and 100F for 9 weeks, and in unlined
tubes at 120F for 9 weeks, exhibit excellent cosmetic stability.
'j
SAL 2
Hydroxyethylcellulose 1.1
, -
I Carbowax owe 20.0
No Saccharin 0.2
, MOP 0.76
CAB (35i10 A 1 547
Dlc~alcium Phosphate : : 46.g
BZCl 0 5
24.0
Flavor 1.0
I!
I
'"I :
'I
-23-
I
,:
, This dental cream is prepared in accordance with the
procedure of Example 1. This product has a pi of 6.7 and a
foam height of 55~ but does not taste good.
EXAMPLE
,
'I=
Hi Sweet peppermint 1.0
MEG 0.1
B~Cl 0
: FOP 0.76
.
:: No Saccharin 0.2
: ' H20 23044
PEW 600Z 20.0
Notoriously 0 :
Jo Dicalcium phosphate 49.0
CAB (30~ AYE.) 4.0
` 1Monoammonium:glycyrrhizinate
Polyethylene glycol~ molecular weight 600
3Hydroxyethylcellulose
: : :
foe I
''
,1 ~24-
, . . .
;
~Z~3~32~
This dental cream it preread according to tic wrecked-
use of Example l, except that the pi is adjusted to I with
dilute Noah for hydration purposes, after the polyethylene
glycol is added to the golfed premix
The resultant cream looks good has a foam height of
3~-409 and show excellent stability using aging tests over a
if
, period of 12 weeks at luff as well as at 140F in unlined tubes
or 3 weeks.
:: :
i, EXAMPLE 4
:
; Example 3: is repeated except that glycerin replaces
Jo : : the polyethylene glycol humectant. This product gives a foam
o
height of 46, but shows trace separation in 3 days at 140 Phoned :;~
:. :a~:wetness:and separation at the neck of the tube at l20F on :
3 weeks. This product is cosmetically unstable.
EXAMPLE 5
:
Ingredients Jo
Ho 21.14
Nutrias 1.3
: Propylene glycol~ : 20.0
:: : :,
! '
25_
!
~23~2~3
;'
1 Ingredients
,.
. No ~ccharin 0.2
B~Cl 0 5
. MUG Cot
MOP 0~76
Dic~lcium phosphate 5~-0
CAB (30~ AYE.) 500
: flavor 1.0
,
. This dental cream is prepared according to the proved-
: Jo ; use of Example l except that the propy}ene~glycol humectant is
: mixed with the premix gel for only lo minutes. The resulting ; product is good in appearance and foaming with a foam height of
44:.~ However its instability is clearly evident by~separa~ion,
wetness along the ribbon and clip leakage in 3 weeks at~F~and~
phoned slight yellowing at 110F and~120F within 3 weeks. :
EXAMPLE 6
,
H20 19.6
Na~rosol Jo
Carbowax 600 ; 20.0
:
.
'
:: :
, :
., ,
~2~82~3;2
Jo
,;
. . .
! No Saccharin 0.2
i BZCl 0~5
MUG Cot
. r p O 76
Dioalcium phosphate 50.0
CAB (owe AYE. ) 6.66
Flavor 1.0
.
This dental cream is prepared according to the proved-
!
; use of example 1.
The resulting product is slightly thick but exhibits
good foaming and stability
. EXAMPLE 7
:
,
1.34
Notoriously
: :Carbowax 600 ; :20.:0:
I: :
No Saccharin : : 0.2
B~Cl : I: 0 5
MAO : 0.1
: 1, :
-27- :
'
~L23
.
,
MOP Owe
. Keep 50~0
.` CAB (owe AYE. ) 5.0
: , flavor 1.0
Calcium pyrophosphate
This dental cream is prepared according to the pro-
seedier of Example 1.
The:resulti~g cream is trick and grainy, which may be
' due Jo the coarseness of the calcium pyrophosphate dental Abram
.. size.
; ; EXAMPLE
: :
O ; ~17.6B
Notoriously 1.1
! :Carbowax 600 20.0
:
,; No Saccharin :0.2
ZCl 0.5
: MUG 0.1
MOP 0.76
:::
;; : :
,:
!
i; :
.1
'I I
i,
Lo 32
;
.
Dicalcium phosphate dehydrate 42.0
An hydrous Dicalcium phosphate 10~0
CAB (owe AYE 6.66
Flavor 1.0
AMPLY 9
Carbowax 600 20~0
: Notoriously 1.1
;; , No Saccharin 0.2 .
.; MUG : - 0.1
BZCl : 0 5:
: H20 : ;;~ 17.6~
; MOP 0~76
: Hydrated Alumina 42.0 : :
Calcined Alumina 10.0
ocoamidopropyl;betaine (kiwi AYE.) :6.66 ; : Jo
Flavor 1.0
Jo : pi : ;: ; :
:
.
i
:
I I:
!
, , :
,/'' ',
I! ,
!
~2~28
I
i This product shows complete stability or aging for
¦ 9 weeks at room temperature 40F, 100F and 120F,
I' .
" ELSE 10 and 11
En. 10 En. 11
. .
PEG 600 20.0 2000
Notoriously tot 1~3
No Saccharin 0.3 0,,3
Hydrated Alumina 42 . 0 42 . 0
:Calcined Alumina 10.0 10.0
CAB (305~ Aye j 5~0 5~0
0.76 0.76
:
Flavor : It 1.0
I: H20 Do 19.27 18064
Equal 0 5 0 5
Red 40 I solution) owe 0.07
:
:
:: :
I 0-
it
l;
EXAMPLE 12
Sorbltol 70/o 2~.0
I Notoriously 1.1
No Saccharin 0.3
BZCl I
MOP 0.76
Alumina 42~0
Calcined Alumina 10.0
CAB (3G~ AYE.) 5.
Flavor 1.0
H 0 11.3
:: :
Initial pi owe
: : 3 we us pi 7.5
6 weeks pi 7.6
;
This product exhibits couplet stability at F and
~0 for appeared ox 9 weeks but slight wet cap at 110F and
120F after 3 9 weeks. In addition to the good physical stability
of this product, the active ingredient content (ionic fluoride
: and the benzethonium chloride) remains stable as evidenced Beth:
substantially stable phi
-31-
I
.. :
EXAMPLE I
.; , %
!'
I. H 0 . 21.1
I, Notoriously 193
Sorbitol 20.0
No Saccharin 0.2
l sly o 5
: : MUG 0.1
0.76
Dicalcium phosphate dehydrate 50~0
:
: : , CAB (~30~ AYE) 500
Flavor 1.0
; I. : ` :
I The resultant cream exhibits a foam height:of~2 and:
; :. no flavor separation after 9 weeks at 120F. This~product;ls : ;
, completely stable at OF and 40F for a period of 9 weeks, but
exhibits traces;of~a~wet cap at phoned 120F after 3: to 9
; weeks.
,
I: :
:
, j
I : :
I : :
. : 32--
,
,;
;
Mull if,.
' ,
.
Notoriously l . l
No Saccharin 0.3
B~Cl owe
MOP 0. 76
Carbowax 600 lo 0
Sorbitol (70~10) Lowe
H20: Donald 19.34
Hydrated Alumina lo 0
Calcined Alumina 42 . 0 : :
Flavor : l . 0 :
CAB owe hi ) 5.0
EXAMPLE 1 5
: I: . :
:: :
Notoriously :
:
No Saccharin Jo 0.3
: MOP ` ; 0.76 :::
: BZCl I: 0.5
Carbowax 600 : l S 0 :
: ~Sorbltol (70~)~ ; 5.0
:
,
I
l,
It ~231~ 2
, . .
i
I go
I
H20 19.34
Hydrated Alumina 42.00
Calcined Alumina 10~0
; Flavor 1 r O
CAB (30~ AYE.) 5~0
This product which contains I sorbitol, exhibits ~410
soluble fluoride recovery at 12 weeks at~100F, as compared to
: owe fluoride recovery (acceptable level) for the polyethylene
glycol humecta~t system alone under the same conditions e.g.
samples l through 11. This indicates that the presence of
: : sorbitol, in amounts as low as owe (owe Ago provides superior
: M uoride stability. : ; :
:
:: : ` :: : : :
,
:: :: :
:: :
:
: : ' :
I
~238~
Examples 16 - 20
% % % % %
Ingredients En. 16 En. 17 En. 18Ex. 19 En. 20
Polyethylene Glycol 15 17 19 10 20
(Carbowax 600)
Glycerin 5 3 1 10 0
Hydroxyethyl Cellulose 1.10 1.10 1.10 1.10 1.10
Sodium Monofluorophosphate 0.76 0.76 0.76 0.76 0.76
Sodium Saccharin 0.30 0.30 0.30 0.30 0.30
B.enzethonium chloride 0.50 0.50 0.50 0.50 0.50
Hydrated Alumina 42 42 42 42 42
Calcined Alumina 10 10 10 10 10
COBB% Awl.) 5 5 5 5 5 I:
Flavor
Water 19.34 19.34 19.34 1~.34 19.34 ;
I content* 0.07 0.067 0.066 0.077 0.057
*Chemical stilt of the above fqr~ulations. after accelerated
aging fur 12 weeks at lQQ as~deter~ined by th.e.~ercentage of
cQnt~nt
-35-
,,
it
If :
I i
Lo
, I ,
; .
ii !
¦¦ All the above formulations are effective against
¦¦ plaque related bacteria while possessing improved foaming
characteristics, cosmetic stability and chemical stability.
The presence ox small amount of glycerin, as low as I by
'White, enhances the chemical stability of the fluoride in the
polyethylene glycol h~u~ectant-containing dentifrice over the
acceptable fluoride stability in the absence of glycerin
(Example 20).
Variations in the above formulations may be made. For
example 9 other buttons such as lauramidopropyl button, coo
; button and the like may be substituted for the oocoamidopropyl
button in the examples. Similarly, other abrasives may be
substituted for the specific abrasives in the examples. Likewise
other fluoride-containing compounds such as sodium fluoride,
potassium fluoride, etc. may be substituted for the sodium
monofluorophosphate in the specific examples. -
: It is understood that the foregoing detailed descrip-
Chinese given merely by way of illustration and what variations
may be made wherein without departing from the spirit of the
invention. the "Abstract" given above is merely or the con-
I
'lenience of ~echnical;searchers and is not to be given any
weight with respect to the scope of the invention.
-36-