Note: Descriptions are shown in the official language in which they were submitted.
` - -
~2749? ~15 48 6 ~
,~.
ORAL CARE PRODUCTS CONTAINING
ZINC-POLYAMINE COMPLEX AND PYROP~OSPE~ATE
CROSS-REFERENCE TO RELATED APPLICATIONS
The subject matter of the present patent
application is related to that disclosed in
U.S. patent application S. N- 08/269,155,
filed June 30, 199~ and U.S. patent application
S.N. 08/26~,15~, - , filed J~ne 30, 1994;
incorporated by reference.
BACKGROUND OF THE INVENTION .
The use of zinc compounds as a source for
physiologically active zinc ions in oral care
products such as mouthwashes, rinses and toothpastes
is a widely accepted practice. Zinc has been used
15 for its ability to neutralize oral malodor, and it
is also recognized that zinc ions have antiplaque
and anticalculus properties.
It is hypothesized that the mechanism of
zinc ions in reducing calculus in dental
20 applications is interference with two stages in the
development of calculus, i.e., the structural
formation of the plaque stage, and the
mineralization of the plaque stage. Both of these
stages normally make the plaque more cohesive, and
25 therefore less permeable to penetration by the
21548~
physiologically active chemical species in the oral
environment. Zinc interferes with the attachment of
the microbial elements to each other and to the
mucilaginous matrix, and also can interfere with the
calcification stage. In both stages the zinc ions
function as an antagonist to calcium ions. It is
postulated that a zinc compound, by preventing the
plaque from becoming dense and strongly cohesive,
causes permeability in the plaque which allows
penetration by the physiologically active antiplaque
and anticalculus ions in the oral environment.
Both water-soluble and water-insoluble
zinc compounds have been utilized as physiologically
active ingredients in oral care preparations.
Water-soluble and highly ionized zinc compounds such
as zinc chloride provide the best source of
bioavailable zinc ions. However, zinc chloride in
aqueous solution tends to form oxychlorides and zinc
hydroxides of low solubility, which results in a
two-phase cloudy solution.
The pH of a conventional zinc chloride
solution can be lowered to less than 4.5 through the
use of mineral or organic acid buffers to provide a
stable and clear solution. However, this method is
not acceptable since the resultant oral care product
exhibits severe astringency and an undesirable sour
taste.
~ f ~
" - -
- 2154~60
Zinc salts such as zinc phenolsulfonate as
disclosed in U.S. 4,022,880, and zinc
carboxymethylsuccinate, as disclosed in
U.S. 4,144,323, tend to be stable at a higher pH
than other zinc salts. Sparingly water-soluble
salts such as zinc citrate have been used to
moderate the release of zinc ions, thereby reducing
astringency and providing a sustained level of
in-vivo anticalculus activity. The use of various
complexing agents such as sodium gluconate
(U.S. 4,568,540), glycine (U.S. 4,339,432 and
U.S. 4,4Z5,325), sodium citrate, citric acid, and
the like, have been employed for production of
relatively stable solutions of zinc chloride.
The reaction or interaction of zinc
compounds of varying solubility with anionic
polymers containing carboxylic, sulfonic and/or
phosphonic acid functionalities are described in
U.S. 4,138,477.
U.S. 4,664,906 describes oral compositions
containing hexedine and a zinc compound which
exhibit antimicrobial activity. Opacified gel
dentifrices are d~sclosed which contain sodium
gluconate and a nonionic binder such as
hydroxyethylcellulose.
U.S. 4,992,2S9 describes a clear aqueous
composition of a zinc salt, a complexing agent such
as succinic acid, and an anionic polymer such as
sodium alginate.
2ls4s6a
` -
Prior art of particular interest with respect to the
present invention subject matter includes United States patent
4,022,880; 4,082,841; and 4,522,806. These references
describe oral care products which contain a zinc compound and
a polyamine compound as two of the formulation ingredients.
There is continuing interest in the development of
new and improved oral care products which retard plaque and
calculus formation in oral cavities.
Accordingly, it is an object of this invention to
provide an oral care product which has superior properties for
controlling plaque, calculus, oral malodor and gingivitis.
It is another object of this invention to provide an
oral care product which slow-releases bioavailable zinc ions
in an oral cavity environment.
It is a further object of this invention to provide
a water-soluble polyamine complex of a normally water-
insoluble zinc compound which has utility as an ingredient of
improved palatability and reduced astringency in oral care
products.
Other objects and advantages of the present
invention shall become apparent from the accompanying
description and examples.
Figure 1 is a graph which represents the mean
salivary zinc concentration vs. time curves for three
dentifrices. The graph comparative data have correspondence
with the dentifrice formulations and procedures described in
Example VII.
65284-78
- 21548~0
DESCRIPTION OF THE INVENTION
One or more objects of the present
invention are accomplished by the provision of an
oral care product which contains an effective
anticalculus mixture of ingredients comprising
(1) about 0.1-15 parts by weight of water-insoluble
zinc compound; (2) about 0.1-15 parts by weight of
water-soluble zinc-complexing polyamine ingredient;
(3) about 0.1-5 parts by weight of alkali metal
pyrophosphate; (4) about 0-5 parts by weight of
surfactant; and (5) about 0-95 parts by weight of
water.
An invention oral care product can be in
the form of a powder essentially free of water, and
the zinc compound ingredient can have an average
particle size between about 0.1-20 microns, and the
alkali pyrophosphate ingredient can have an average
particle size between about 5-600 microns.
When an invention oral care product has a
water content between about 12-95 parts by weight,
the zinc compound is in the form of a water-soluble
zinc-polyamine complex. An invention oral care
product typically is a toothpaste or mouthwash
formulation.
The term "single-phase" as employed herein
refers to an invention aqueous solution which has a
clear transparency, without any visible evidence of
a second phase which is distinct from the aqueous
phase. The aqueous solution contains zinc compound
and polyamine in the form of a water-soluble zinc-
polyamine complex.
2154860
The term "water-insoluble" as employed
herein refers to a zinc-containing compound which
has a solubility in water that is equivalent to less
than about 0.5 gram of zinc ions in 100 milliliters
S of water at 25C. The slight solubility of the zinc
compound in water is sufficient to slow-release
bioavailable zinc ions in an oral environment.
The term "water-soluble" as employed
herein refers to polyamines which have a solubility
of at least about two grams per 100 milliliters of
water at 25C.
An invention oral care product has an
effective anticalculus content of zinc compound,
such as between about 0.05-5 weight percent, based
on the oral product weight.
Zinc compounds having a solubility which
provides less than about 0.5 gram of bioavailable
zinc ions per 100 milliliters of water at 25C, and
which are suitable as an ingredient in an invention
oral care product, include zinc oxide, zinc
silicate, zinc carbonate, zinc tetrafluoroborate,
zinc hexafluorosilicate, zinc citrate, zinc
benzoate, zinc oxalate, zinc stearate, and the like.
Polyamines which are suitable as an
ingredient in an invention oral care product include
water-soluble chemical structures which have at
least 4 amine groups such as polyalkylenamines
- 21~4~6Q
having a weight average molecular weight between
about 800-1,000,000. A preferred type of
polyalkylenamine is one which corresponds to the
formula:
R
[ (CH2) n~N ]
where R is a hydrogen, Cl-C3 alkyl or t (CH2)n-NH-~-
substituent, and n is an integer in the range of
2-6.
A polyamine ingredient can contain other
heteroatoms such as oxygen and sulfur. The amine
groups can be any combination selected from primary,
secondary and tertiary amine structures. The
polyamine ingredient must have sufficient amine
basicity to coordinate with the zinc compound and
form a water-soluble zinc-polyamine complex.
Another type of polyamine which can be
employed as a zinc-complexing ingredient in an
invention aqueous solution is a basic aminoacid
polymer having a weight average molecular weight
between about 1500-70,000. Illustrative of these
aminoacid polymers are polyarginine, polylysine and
polyhistidine.
\ - -
- 2154860
A present invention oral care product can
be prepared conveniently by dissolving the polyamine
ingredient in an aqueous medium, and then adding the
zinc compound in powder form to the aqueous solution
with stirring to form a zinc-polyamine complex.
Solubilizing of the zinc compound in the aqueous
polyamine solution also can be facilitated by
employing an ultrafine powder form. Zinc oxide
having an average particle size less than about five
microns is a commercially available product.
After completion of the zinc compound
addition, the resultant single-phase clear aqueous
solution can have a pH above about 10 because of the
polyamine basicity. Preferably, an acid reagent
such as hydrochloric acid is added to adjust the
aqueous solution pH into the range between about
6-10.
A pH above about 10 can have an irritating
effect on sensitive membranes when an oral care
product containing the aqueous solution is used in a
dental application. A pH below about 6 can cause
acid etching of tooth enamel. It is advantageous to
maintain the aqueous zinc-polyamine complex solution
pH in the 6-10 range.
The aqueous zinc-polyamine complex
solution can be incorporated as a component of
invention oral care products such as toothpastes and
mouthwashes. A typical oral care product will have
a zinc ion concentration between about
0.05-2.0 weight percent.
215~86~
A toothpaste formulation can be prepared
by blending a present invention aqueous solution of
zinc-polyamine complex with the pyrophosphate
ingredient, and other conventional ingredients which
are employed as adjuvants in oral care products.
Suitable alkali metal pyrophosphates
include dialkali metal and tetraalkali metal
pyrophosphate and mixtures thereof in a hydrated or
unhydrated form. Illustrative of pyrophosphate
salts are Na2H2P207, Na4P207 and K4 2 7
Suitable adjuvants include whitening
agents such as titanium dioxide; preservatives;
silicones; chlorophyll compounds; peroxygen
compounds such as sodium percarbonate; antibacterial
agents such as cetyl pyridinium chloride; flavorants
such as oils of spearmint and peppermint; sweetening
agents such as sucrose and sodium cyclamate;
fluoride compounds such as sodium fluoride and
sodium monofluorophosphate; humectants such as
glycerin; gelling agents such as sodium
carboxymethylcellulose; abrasives such as alpha-
alumina, particulate polyvinyl chloride, calcium
phosphate, silica xerogel and sodium bicarbonate;
and the like.
- 2154860
Other adjuvants employed in toothpaste
formulations include between 0.05-S parts by weight
of a surfactant such as cetyltrimethylammonium
bromide; sodium lauryl sulfate; sodium
dodecylbenzenesulfonate; ammonium lignosulfonate;
condensation products of ethylene oxide with fatty
alcohols, amines or alkylphenols; partial esters of
fatty acids and hexitol anhydrides; and the like.
A mouthwash formulation can be prepared by
blending a present invention aqueous solution of
zinc-polyamine complex with other ingredients of the
type described above, which include aqueous ethanol,
glycerin, sorbitol, surfactant, colorant, flavorant,
antibacterial agent, and the like.
By the practice of the present invention,
an oral care product can be prepared which has
superior properties for retarding plaque and
calculus formulation, and controlling bad breath and
gingivitis. Important advantages derive from the
presence of a present invention zinc-polyamine
complex as a component of an oral care product, when
the oral care product is applied to an oral cavity
following a prescribed regimen.
A present invention zinc-polyamine complex
can be adsorbed onto oral surfaces. The zinc-
polyamine complex provides a means of attachment in
the oral cavity, and functions as a reservoir of
2154860
zinc ions which are sustained-released over an
extended time period and are effective for
controlling plaque, calculus, mouth odor and
gingivitis.
As a further advantage, the zinc-polyamine
complex is in a form that decreases the astringency
which is characteristic of zinc ions, and thereby
leaves a more pleasant taste in the mouth.
The following examples are further
illustrative of the present invention. The
components and specific ingredients are presented as
being typical, and various modifications can be
derived in view of the foregoing disclosure within
the scope of the invention.
` -
21~48SO
EXAMPLE I
This Example illustrates the preparation
of a present invention aqueous solution containing a
zinc-polyamine complex.
InqredientsParts By Weiqht
Polymin p(1) 12
hydrochloric acid (50% aq. sol.) 21
zinc oxide powder 4
distilled water to lO0
lO The polyamine is dissolved in about
50 parts of distilled water. The zinc oxide powder
is added to the aqueous solution, and stirring is
continued for about 30 minutes. Hydrochloric acid
solution is added to adjust the pH to 7-8.
Distilled water is added to lO0 parts by weight.
The final aqueous solution is a single
phase transparent medium with a pH of 7-8.
A similar solution of zinc-polyamine
complex is obtained when zinc citrate is employed
instead of zinc oxide.
PEI 1500 (CTFA) ; polyethylenimine
(M.W. 75,000; BASF)
- 215~860
EXAMPLE II
This Example illustrates comparative data
which demonstrate that a present invention aqueous
zinc-polyamine complex solution exhibits an enhanced
anticalculus effect.
Anticalculus evaluation is conducted with
an in-vitro method similar to that described in
J. Clin. Den., 2, 48 (1990) by Schiff & Volpe. A
higher T1 value represents a greater anticalculus
effect.
The comparative data are summarized in the
following Table:
2l~4a6~
TABLE
Aqueous Systems Tl, minutes
1. distilled water control 14.25
2. 2% zinc oxide aqueous suspension 15.00
3. 6% PEI(l) 14.25
4. 0.25% PEI + 2.0% zinc oxide 16.00
5. 0.25% PEI + 4.0% zinc oxide 16.00
6. 2.0% PEI + 2.0% zinc oxide 21.00
7. 2.0% PEI + 4.0% zinc oxide 21.50
8. 5.0% TSPP(2) aqueous solution 23.00
9. Colgate TC 20.00
10. 6% PEI + 2% zinc oxide 26.50
11. Crest TC 27.75
12. 5.0% zinc citrate(3) 17.25
13. 5.0% zinc citrate + 2% PEI 25.75
14. 2.0% PEI + 4.0% zinc oxide + 2.0% TSPP 32.00
15. 6.0% PEI + 2.0% zinc oxide + 5.0% TSPP 50.25
(1) Polymin P (M.W. 75,000; BASF); PEI 1500 (CTFA)
'2) tetrasodium pyrophosphate
(3) 2% zinc oxide and 5% zinc citrate are equivalent
in zinc molarity
- 2~5~6~
EXAMPLE III
This Example illustrates the preparation
of a dentifrice composition which contains
tetrasodium pyrophosphate and an aqueous solution of
a zinc-polyamine complex in accordance with the
present invention.
InqredientsParts By Weiqht
glycerin 15.00
PEG-8(1) 1.00
10 sodium carboxymethylcellulose gum0.60
sorbitol (70~ soln.) 27.56
distilled water 10.00
sodium fluoride 0.24
hydrated silica 16.00
zinc-PEI 1500 solution (Example I)25.00
tetrasodium pyrophosphate 2.00
sodium lauryl sulfate 1.20
sodium saccharin 0.50
flavor oil 0.90
(1) polyethylene glycol (M.W. 400)
2~ 6a
The sodium carboxymethylcellulose,
glycerin and PEG-8 ingredients are admixed with
stirring to form a suspension. Sorbitol and sodium
fluoride (in aqueous solution) are added to the
suspension, and stirring is continued for about
30 minutes. Hydrated silica is added with stirring,
followed by the addition of the zinc-PEI solution
with stirring for about 10 minutes. Tetrasodium
pyrophosphate, sodium lauryl sulfate and flavor oil
are blended into the admixture to form a homogeneous
toothpaste formulation. The product is deaerated
and filled into tubes.
~1~4~6Q
EXAMPLE IV
This Example illustrates the preparation
of a mouthwash formulation which contains
tetrasodium pyrophosphate and an aqueous solution of
a zinc-polyamine complex in accordance with the
present invention.
Ingredients Parts By Weiqht
distilled water 56.09
glycerin 11.00
SD alcohol 38-B~1) 5.00
zinc-PEI 1500 solution (Example I) 25.00
sodium benzoate . 0.20
sodium saccharin 0.50
tetrasodium pyrophosphate 1.00
Poloxamer 407~2) 0.60
flavor oil 0.60
FD&C Blue #1 0.01
~1) denatured ethanol
'2) polyoxyethylene-polyoxypropylene block polymer
2~86a
18
The distilled water, glycerin and zinc-
polyamine complex solution are admixed to form an
aqueous solution. The sodium benzoate, sodium
saccharin, tetrasodium pyrophosphate and colorant
are added to the aqueous solution with stirring.
The alcohol, flavorant and Poloxamer 407
ingredients are preblended, and the blend is added
to the aqueous solution with stirring to form a
clear blue mouthwash formulation.
`- 2l5~86~
19
EXAMPLE V
This Example illustrates the preparation
of toothpaste formulations containing zinc-polyamine
complex, sodium bicarbonate and tetrasodium
pyrophosphate ingredients in accordance with the
present invention.
Ingredients Parts By Weiqht
a b c
glycerin 14.070 14.070 14.070
PEG-8 1.000 1.000 1.000
sodium carboxymethylcellulose 0.850 0.850 0.850
distilled water ; 11.687 17.687 21.062
sodium fluoride 0.243 0.243 0.243
sodium saccharin 1.200 1.200 1.200
sodium bicarbonate 57.250 55.000 55.000
PEI 1500 (50% soln.) 4.000 2.000 1.000
hydrochloric acid (50% soln.) 3.500 1.750 0.875
zinc oxide 2.000 2.000 0.500
tetrasodium pyrophosphate2.000 2.000 2.000
sodium lauryl sulfate 0.300 0.300 0.300
sodium lauroyl sarcosinate1.000 1.000 1.000
(30% soln.)
flavorant o.goo o.goo o.goo
TOTAL 100.000 100.000 100.000
- 21~ ~86~
The glycerin, PEG-8 and sodium
carboxymethylcellulose are admixed, followed by the
addition of aqueous sodium fluoride solution.
Sodium saccharin and sodium bicarbonate are added to
the admixture with stirring. Separately, the
tetrasodium pyrophosphate is preblended with the
PEI 1500, zinc oxide, 50% HCl and distilled water,
and the blend is added to the main admixture. The
final product is obtained by adding sodium lauryl
sulfate, sodium lauroyl sarcosinate and flavorant to
the admixture and stirring to form a homogeneous
toothpaste formulation.
- ~15~86~
EXAMPLE VI
This Example illustrates the preparation
of gel toothpaste formulations containing zinc-
polyamine complex, sodium bicarbonate and
tetrasodium pyrophosphate ingredients in accordance
with the present invention.
Ingredients Parts By Weight
a b c
glycerin 10.000 10.000 10.000
sorbitol (70% soln.)23.000 23.000 23.000
PEG-8 1.000 1.000 1.000
sodium carboxymethylcellulose 0.650 0.650 0.650
distilled water 7.337 11.087 14.462
sodium fluoride 0.243 0.243 0.243
sodium saccharin 0.500 0.500 0.500
sodium bicarbonate 30.000 30.000 30.000
hydrated silica 12.500 12.500 12.500
PEI 1500 (50% soln.) 4.000 2.000 1.000
hydrochloric acid (50~ soln.) 3.500 1.750 0.875
zinc oxide 2.000 2.000 0.500
tetrasodium pyrophosphate2.000 2.000 2.000
sodium lauryl sulfate 0.500 0.500 0.500
sodium lauroyl sarcosinate1.670 1.670 1.670
(30% soln.)
flavorant 0.900 0.900 0.900
FD&C Blue #1 (1% soln.)0.167 0.167 0.167
D&C Yellow #10 (1% soln.)0.033 0.033 0.033
TOTAL 100.000 100.000 100.000
2154~6~
Following the procedure described in
Example V, the above ingredients are blended in the
approximate order listed. The final homogeneous gel
formulations are deaerated and filled into standard
toothpaste tubes.
~15~860
EXAMPLE VII
This Example illustrates the increased
oral retention of zinc with a toothpaste dentifrice
which contains zinc compound and polyamine
ingredients in accordance with the present
invention.
Comparative salivary tests are conducted
to determine the effect of polyethylenimine on the
salivary clearance of zinc oxide delivered from a
sodium bicarbonate-containing dentifrice.
Dentifrices containing 59.25% sodium
bicarbonate and 2% zinc oxide with and without
2% polyethylenimine are prepared, with complete
formulations as shown in Table 1. A commercial
dentifrice containing 1% zinc citrate trihydrate
(ZnCit) also is tested (Close-Up Tartar Control
Gel).
The three zinc-containing dentifrice
products are tested in a blind cross-over brushing
design. Six human subjects are recruited, and they
abstain from all oral hygiene on the morning of each
test. Only one product per day is tested, and the
subjects are blinded to the identity of the
products. On the day of testing, an unstimulated
saliva sample is obtained from each subject prior to
brushing. The subjects brush with 2 g of a test
product for 60 seconds and rinse for 5 seconds with
215~8~0
15 ml of distilled water. Following rinsing,
unstimulated saliva samples are collected at 1, 5,
10, 15, 30, 45 and 60 minutes. During this period
the subjects refrain from eating, drinking or gum
chewing, and minimize talking. After sample
collection, 0.4 ml of each saliva sample is diluted
with 5 ml 1 N HCl in polypropylene vials. The
diluted samples are mixed using a vortex mixer, and
analyzed for zinc using ICP spectrophotometry.
The mean salivary zinc concentration vs.
time curves for the three test dentifrices are shown
in Figure 1. Prior to brushing, the mean baseline
salivary zinc concentrations are 0.56, 0.41 and
0.59 ~g Zn/ml saliva for the ZnO, ZnO/PEI 1500 and
commercial zinc citrate dentifrices (ZnCit),
respectively. The salivary clearance curves for the
test products exhibit a typical biphasic salivary
clearance pattern. This is characterized by a rapid
initial decline in salivary zinc followed by a
slower secondary elimination of zinc from saliva.
The salivary zinc levels for all
dentifrice products as expected is highest
immediately following the water rinse. At 1 minute
post-brushing, the mean salivary zinc concentrations
are 111, 129 and 44 ~g Zn/ml for the ZnO, ZnO/PEI
1500 and ZnCit dentifrices, respectively. At
5 minutes, the mean salivary zinc levels are 39, 48
215~0
and 15 ~g Zn/ml, respectively. Differences between
products at 1 and 5 minutes post-brushing are due to
differences in product zinc concentrations. The
ZnCit dentifrice contains 1.0% zinc citrate
trihydrate, which is equivalent to about 0.31% Zn or
0.39~ ZnO. In comparison, the ZnO dentifrices
contain 2.0% ZnO. While higher initial
concentrations of zinc are obtained as a result of
increased levels of zinc in the ZnO dentifrices, the
effect is transitory and not sustained beyond
5 minutes post-brushing.
The mean salivary zinc levels at
10 minutes post-brushing decreased to 13, 18 and
9 ~g Zn/ml respectively for the ZnO, ZnO/PEI and
ZnCit dentifrices. These levels are not
significantly different from each other (p>0.05).
At 15 to 60 minutes post-brushing, the ZnO/PEI 1500
dentifrice provides significantly (p<0.05) higher
mean salivary zinc levels then either the ZnO or
ZnCit dentifrices. The ZnO/PEI lSOO dentifrice
provides mean salivary zinc concentrations ranging
between 10 to 18 ~g Zn/ml during the 15 to
60 minutes post-brushing. In comparison, the ZnCit
dentifrice provides mean salivary zinc
concentrations ranging from 4 to 6 ~g Zn/ml.
Similarly, the mean salivary zinc concentration
21~48~0
26
provided by the ZnO dentifrice drops from 7 ~g Zn/ml
at 15 minutes to less than 2 ~g Zn/ml at 60 minutes.
There are no differences between the ZnCit and the
ZnO dentifrices during this time period. A
statistical summary of the data is illustrated in
Table 2.
The salivary test data indicate that zinc
can be delivered at a high level to the oral cavity
from a zinc oxide baking soda dentifrice, and that
the addition of PEI 1500 significantly increases the
oral retention of zinc. This delivery and retention
directly relates to the beneficial bioactivity of
zinc, since the bioactivity of an oral antimicrobial
agent is dependent upon the delivery of an effective
concentration, i.e., the dosage, frequency of
application, and retention of the agent within the
oral cavity.
During the saliva collection periods, five
of the six subjects offer comments that the
aftertaste of the commercial zinc citrate dentifrice
is objectionable. The metallic aftertaste and high
degree of astringency are the most prevalent
observations. The metallic taste and astringent
feeling of soluble and partially soluble zinc salts
is well-known. The magnitude of these perceptions
is dependent upon zinc concentration. Although the
21~48~Q
ZnO/PEI 1500 dentifrice provides a higher sustained
level of salivary zinc, no subject finds this
product to possess any objectional metallic or
astringent aftertaste as is noted with the ZnCit
product. The PEI 1500 appears to moderate the taste
perception of zinc.
2l5~86~)
TABLE I
ZINC OXIDE DENTIFRICES WITH AND WITHOUT PEI 1500
Parts By Weiqht
INGREDIENT ZnOZnO/PEI 1500
Zinc oxide
(Sachtleben Chemie)2.000 2.000
PEI 1500 0.000 4.000
(50% soln., Polymin P;
BASF)
50% HCl (6N HCl) 0.000 3.500
Distilled water 19.173 11.673
Sodium bicarbonate59.250 59.250
Glycerin (99.7%)14.070 14.070
PEG-8 (Carbowax 400;1.000 1.000
Union Carbide)
Sodium carboxymethyl-0.850 0.850
cellulose
Sodium fluoride 0.243 0.243
Sodium saccharin 1.208 1.208
Sodium lauryl sulfate0.300 0.300
Hamposyl L-30 (Grace)(1) 1.000 1.000
Flavor (H&R 9377)0.906 0.906
Total 100.000 100.000
(1) Sodium lauroyl sarcosinate.
- 21~486~
TABLE 2
STATISTICAL SUMMARY OF RESULTS*
TEST PRODUCT1-5 mins. 10 mins. 15-60 mins.
ZnO/PEI dentifrice A B
A B
ZnO dentifrice A B C
B C
Close Up (Zn Citrate) B C
*Products with the same letter are not statistically
different (p<0.05) within the specified time period.
