U.S. patent application number 10/015964 was filed with the patent office on 2002-11-07 for stable emulsions for cosmetic products.
This patent application is currently assigned to Colgate-Palmolive Company. Invention is credited to Brahms, John, Bustos, Mardoqueo, Chopra, Suman Kumar, Hilliard, Peter JR., Johansson, Marie, Moghe, Bhal, Ortiz, Claudo, Popoff, Christine, Schamper, Thomas.
Application Number | 20020164296 10/015964 |
Document ID | / |
Family ID | 24300498 |
Filed Date | 2002-11-07 |
United States Patent
Application |
20020164296 |
Kind Code |
A1 |
Schamper, Thomas ; et
al. |
November 7, 2002 |
Stable emulsions for cosmetic products
Abstract
Low water emulsions are described which are useful for
antiperspirants and/or deodorants wherein the emulsions are made by
combining (I) 15-33% of an external phase comprising: (a) 1-25% of
an organic ester having a refractive index in the range of
1.43-1.60 and capable of releasing an antiperspirant active to
achieve a specified conductivity; (b) a sufficient amount of a
silicone copolyol to achieve a solids content of 0.25-10%; (c) a
sufficient amount of a volatile silicone to achieve a total amount
of the external phase as 15-33%; (c) 0-5% of a silicone elastomer
(on an actives basis); and (d) 0-15% of at least one emollient; and
(II) 67-85% of an internal phase comprising: (a) an effective
amount of at least one cosmetically active ingredient; (b) a
sufficient amount of a solvent component to dissolve the
cosmetically active ingredient with a maximum amount being about
80%; (c) 0.5-15% of water optionally containing up to 30% of an
ionizable salt soluble in water; (d) 0-5% of a non-ionic
emulsifier; and (e) 0-10% ethanol; wherein: (1) the final
refractive index of the composition is in the range of 1.42-1.52;
and (2) the conductance of the composition is at least 250 micro
Siemens/cm/ml at a loading of at least 7% by weight level of
antiperspirant active.
Inventors: |
Schamper, Thomas; (Cranbury,
NJ) ; Chopra, Suman Kumar; (Dayton, NJ) ;
Moghe, Bhal; (Whitehouse Station, NJ) ; Brahms,
John; (Piscataway, NJ) ; Bustos, Mardoqueo;
(Hillsborough, NJ) ; Hilliard, Peter JR.; (Far
Hills, NJ) ; Johansson, Marie; (Watchung, NJ)
; Ortiz, Claudo; (Dayton, NJ) ; Popoff,
Christine; (Mornganville, NJ) |
Correspondence
Address: |
Colgate-Palmolive Company
Patent Department
909 River Road
P.O. Box 1343
Piscataway
NJ
08855-1343
US
|
Assignee: |
Colgate-Palmolive Company
|
Family ID: |
24300498 |
Appl. No.: |
10/015964 |
Filed: |
December 13, 2001 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
|
|
10015964 |
Dec 13, 2001 |
|
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09575483 |
May 19, 2000 |
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6403067 |
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Current U.S.
Class: |
424/65 |
Current CPC
Class: |
A61K 8/06 20130101; A61Q
15/00 20130101; A61K 8/894 20130101 |
Class at
Publication: |
424/65 |
International
Class: |
A61K 007/32 |
Claims
We claim:
1. A low water emulsion made by combining 15-33% of an external
phase and 67-85% of an internal phase wherein: (I) the external
phase comprises: (a) 1-25% of an organic ester having a refractive
index in the range of 1.43-1.60 and which allows the release of an
antiperspirant active; (b) a sufficient amount of a silicone
copolyol to achieve a solids content of 0.25-10%, wherein the
silicone copolyol may be added with or without solvent; (c) a
sufficient amount of a volatile silicone to achieve a quantum
sufficient amount of the external phase as 15-33%; (d) 0-5% of a
silicone elastomer (on an actives basis); and (e) 0-15% of at least
one emollient. (II) the internal phase comprises: (a) an effective
amount of at least one cosmetically active ingredient selected from
the group consisting of 0.1-25% of an antiperspirant active (on an
anhydrous basis), 0.1-3% of a fragrance, and 0.05-5% of an
antimicrobial; (b) a sufficient amount of a solvent component to
dissolve the cosmetically active ingredient and to complete the
internal phase up to a maximum of 80% of solvent; (c) 0.5-15 % of
water optionally containing up to 30 % of an ionizable salt soluble
in water; (d) 0-5 % of a non-ionic emulsifier; and (e) 0-10%
ethanol; wherein: the final refractive index of the composition is
in the range of 1.42-1.52; the composition is free of borate
crosslinkers; and all amounts are in percent by weight based on the
entire weight of the composition.
2. A low water emulsion as claimed in claim 1 wherein the minimum
conductance at least 250 micro Siemens/cm/ml at a loading of at
least 7% by weight level of antiperspirant active.
3. A low water emulsion as claimed in claim 1 wherein the minimum
conductance is at least 300 micro Siemens/cm/ml at a loading of at
least 7% by weight level of antiperspirant active.
4. A low water emulsion as claimed in claim 1 wherein the minimum
conductance is at least 400 micro Siemens/cm/ml at a loading of at
least 7% by weight level of antiperspirant active.
5. A low water emulsion as claimed in claim 1 wherein the organic
ester is selected from the group consisting of esters of formula
R"--CO(O)--R', where each of R' and R" is independently selected
from the group consisting of (a) C1-C30- straight and branched
chain alkyls and alkenyls; and (b) an aromatic group such as
phenyl, benzyl, naphthyl, or biphenyl wherein the aromatic is
optionally substituted by one or more or the groups listed in (a),
but provided that the total of the carbons for R'+R" is in the
range of 8-30.
6. A low water emulsion as claimed in claim 1 wherein the organic
ester is selected from the group consisting of C12-15 alkyl
benzoate; octyl methoxy cinnamate in amounts less than 6%;
isostearyl isostearate; benzyl benzoate;
2,6-di-(ethylhexyl)naphthalate; butyl octyl salicylate; glyceryl
monostearate; n-dibutyl sebacate; isopropyl myristate; isopropyl
palmitate; butyl stearate; cetyl lactate; isocetyl stearate; hexyl
laurate; decyl oleate; isostearyl isostearate; ethyl hexyl maleate;
sorbitan monoaurate; sorbitan monooleate; sorbitan sesquioleate;
sorbitan trioleate; isopropyl palmitate; isopropyl stearate;
stearyl stearate; disopropyl adipate; diisopropyl sebacate; butyl
myristate; and isopropyl laurate.
7. A low water emulsion as claimed in claim 1 comprising a
sufficient amount of a silicone copolyol to achieve a solids
content of 1.0-3.0%.
8. A low water emulsion as claimed in claim 1 wherein a refractive
index is obtained for each of the external and internal phases and
the refractive indices of the external and internal phases are
matched within 0.01 to obtain a clear product.
9. A low water emulsion as claimed in claim 1 wherein the emulsion
is an antiperspirant.
10. A low water emulsion as claimed in claim 1 wherein the emulsion
is a deodorant.
11. A low water emulsion as claimed in claim 1 comprising up to 30%
of an ionizable salt soluble in water.
12. A low water emulsion as claimed in claim 11 wherein the
ionizable salt is selected from the group consisting of salts of
the form M.sub.aX.sub.b where a=1 or 2; b=1 or 2; M is a member
selected from the group consisting of Nan.sup.+1, Li.sup.+1,
K.sup.+1, Mg.sup.+2, Ca.sup.+2, Sn.sup.+2, and Zn.sup.+2; and X is
a member selected from the group consisting of chloride, bromide,
iodide, citrate, gluconate, lactate, glycinate, glutamate,
ascorbate, aspartate, nitrate, phosphate, hydrogenphosphate,
dihydrogenphosphate, formate, malonate, maleate, succinate,
carbonate, bicarbonate, sulfate and hydrogensulfate.
13. A low water emulsion as claimed in claim 12 wherein the
ionizable salt is selected from the group consisting of NaCl, KCl,
ZnCl.sub.2, zinc citrate and zinc glycinate.
14. A low water emulsion as claimed in claim 1 further comprising
up to 5% of a non-ionic emulsifier.
15. A low water emulsion as claimed in claim 1 further comprising
up to 10% of ethanol.
16. A low water emulsion as claimed in claim 1 wherein refractive
index of the emulsion is in the range of 1.42-1.52.
17. A low water emulsion as claimed in claim 1 wherein the solvent
is a glycol or polyglycol selected from the group consisting of
ethylene glycol, propylene glycol, 1,2-propanediol, diethylene
glycol, triethylene glycol, tetraethylene glycol, dipropylene
glycol, tripropylene glycol, methyl propanediol, 1,6-hexanediol,
1,3-butanediol, 1,4-butanediol, PEG-4 through PEG-100, PPG-9
through PPG-34, pentylene glycol, neopentyl glycol,
trimethylpropanediol, 1,4-cyclohexanedimethanol,
2,2-dimethyl-1,3-propanediol,
2,2,4,4-tetramethyl-1,3-cyclobutanediol, and mixtures thereof.
18. A low water emulsion as claimed in claim 17 wherein the solvent
is a glycol or polyglycol selected from the group consisting one or
more members of the group consisting of propylene glycol,
dipropylene glycol, tripropylene glycol, 2-methyl-1,3-propanediol,
methyl propylene glycol, low molecular weight (less than 600)
polyethylene glycol, low molecular weight (less than 600)
polypropylene glycols, and mixtures of any of the foregoing.
19. A low water emulsion as claimed in claim 1 wherein the
antimicrobial agent is selected from the group consisting of
bacteriostatic quaternary ammonium compounds; 2, 4,
4'-trichloro-2'-hydroxydiphenylether;
N-(4-chlorophenyl)-N'-(3,4-dichlorophenyl)urea; silver halides;
octoxyglycerin and bacteriostatic zinc salts.
20. A low water emulsion as claimed in claim 9 wherein (I) the
external phase comprises: (a) 5-15% of the organic ester; (b)
3.0-6.0 of a 48% dimethicone copolyol or its equivalent; (c) 5-15%
of a volatile silicone; (d) 0-5% of a silicone elastomer (actives
basis); (II) the internal phase comprises: (a) 7.0-25% of an
antiperspirant active (on an anhydrous basis); (b) 35-55% of a
solvent component which comprises at least one glycol; (c) 2-13%
water; (d) 0-5% nonionic emulsifier; (e) 0-3% NaCl; (f) 0-10%
ethanol or its equivalent; and (g) 0-3% fragrance.
21. A low water emulsion as claimed in claim 10 wherein (I) the
external phase comprises: (a) 5-15% of the organic ester; (b)
3.0-6.0 of a 48% dimethicone copolyol or its equivalent; (c) 5-15%
of a volatile silicone; (d) 0-5% of a silicone elastomer (actives
basis); (II) the internal phase comprises: (a) up to 7.0% of an
antiperspirant active (on an anhydrous basis); (b) 40-80% of a
solvent component which comprises at least one glycol; (c) 2-13%
water; (d) 0-5% nonionic emulsifier; (f) 0-3% NaCl; (g) 0-10%
ethanol; (h) 0-3% fragrance.
22. A low water emulsion as claimed in claim 20 or claim 21 wherein
the organic ester is C12-15 alkyl benzoate.
23. A low water emulsion as claimed in claim 20 or claim 21
comprising 2-7% water.
24. A low water emulsion as claimed in claim 1 or claim 11 wherein
the internal phase additionally comprises a member selected from
the group consisting of urea, guanidine hydrochloride, xylitol,
trehalose, maltose and glycerine.
Description
FIELD OF THE INVENTION
[0001] This invention relates to stabilized cosmetic products,
especially antiperspirant and/or deodorant products which may
include an antiperspirant active ingredient and a low water
component which provides better efficacy and stability without
compromising aesthetics. The compositions are emulsions made with
an external (or oil) phase and an internal phase which contains the
active ingredient. These emulsions may be used to form gel, soft
solid or roll-on products.
BACKGROUND OF THE INVENTION
[0002] A large variety of antiperspirant and/or deodorant
formulations have been described in the patent literature and/or
have been made commercially available. These products have included
suspension as well as emulsions. Also various physical forms may be
used such as solids (for example, wax and gel sticks), semi-solids
(for example, gels and creams), liquids (for example, roll-on
products) and sprays (both aerosol and non-aerosol). In recent
years a strong emphasis has been placed on improving both the
performance and the aesthetics of these products. One of the
particular problems is trying to obtain an emulsion product that
has efficacy comparable to suspension products. A second problem is
the stabilization of emulsion products to achieve a product that is
shelf stable, but which releases an active ingredient in a timely
manner.
[0003] With regard to emulsions, U.S. Pat. No. 4,673,570 to Soldati
describes uniform, clear gelled antiperspirant compositions, free
of waxes wherein the emulsions comprise in combination a volatile
silicone fluid, a silicone emulsifier (such as a mixture of
cyclomethicone and dimethicone copolyol), a destabilizing auxiliary
emulsifier, water, a non-volatile emollient (such as C10-C20 alkyl
fatty esters and ethers), linear silicone fluids, a coupling agent
(such as low molecular weight alcohols and glycols), an active
antiperspirant component and other ancillary agents.
[0004] U.S. Pat. No. 5,008,103 to Raleigh et al describes
water-in-oil antiperspirant emulsions having a discontinuous polar
phase containing water and optionally containing an emulsifier with
a hydrophilic-lipophilic balance (HLB value) greater than 8, and a
volatile silicone continuous phase with a dimethicone copolyol
emulsifier. The HLB parameter is a well known parameter the
calculation of which is disclosed and explained in numerous
references. For nonionic surfactants, data obtained by actual
analysis is usually a more accurate measure of HLB values (rather
than theoretical determinations). For purposes of this invention it
is intended that either the actual or theoretical HLB value may be
used as the basis for selection. U.S. Pat. No. 5,401,870 to Raleigh
et al and U.S. Pat. No. 5,292,503 to Pereira et al describe similar
subject matter.
[0005] U.S. Pat. No. 5,216,033 to Pereira et al describes a
transparent water-in-oil emulsion containing a silicone phase with
a dimethicone copolyol and an aqueous phase containing a refractive
index "transparency structurant" to produce a refractive index
matched clear emulsion. The transparency structurant is a C3-C8
polyhydric alcohol.
[0006] U.S. Pat. No. 5,599,533 to Stepniewski et al describes the
use of silicone elastomer in an aqueous water-in-oil emulsion, but
does not describe a clear emulsion.
[0007] U.S. Pat. No. 5,989,531 describes a liquid composition made
with (a) an active phase comprising a selected glycol, a nonionic
emulsifier having an HLB value greater than 8 and an antiperspirant
and/or deodorant active; and (b) a silicone phase made with one or
more of a dimethicone copolyols having an HLB less than 7 and
nonionic emulsifiers having an HLB greater than 7, wherein the
silicone phase has at least 10% silicone and the ratio of the
silicone phase to he active phase is in the range of 1:1-1:4.
Optional ingredients include the use of non-volatile silicones,
volatile silicones and organic emollients.
[0008] U.S. Pat. No. 6,010,688 discloses the use of polyhydric
alcohols to improve the stability and efficacy of antiperspirant
formulations, particularly antiperspirant gels.
[0009] U.S. Pat. No. 5,955,065 discloses antiperspirant gel
compositions containing soluble calcium salts. These compositions
contain an aluminum or aluminum-zirconium antiperspirant salt and a
water soluble calcium salt, both of which are suspended in a
dermatologically acceptable anhydrous carrier vehicle. The present
invention also embraces a method of inhibiting or reducing
perspiration by topically applying an effective amount of such an
antiperspirant composition to the skin.
[0010] U.S. Pat. No. 5,925,338 discloses a clear antiperspirant or
deodorant gel composition which exhibits reduced staining while
retaining excellent aesthetic attributes and efficacy. The oil
phase comprises about 10 to 25% of the composition and contains a
silicone oil and a polyether substituted silicone emulsifying
agent. The silicone oil comprises a mixture of a non-volatile
silicone, preferably a non-volatile linear silicone, and a volatile
linear silicone. It has been found that reducing the amount of
non-volatile silicone in the known gel composition to a relatively
low level (e.g. below about 5%) and adding an amount of volatile
linear silicone to the composition (e.g. above about 2%, preferably
above about 5%) substantially improves the non-staining properties
of the composition.
[0011] U.S. Pat. No. 5,623,017 discloses a clear silicone gel
cosmetic composition with a water-containing internal phase. The
silicone emulsifiers discussed are non-polymeric ethoxylated
bis-trisiloxanes.
[0012] U.S. Pat. No. 6,007,799 discloses a clear cosmetic gel
composition in the form of a water-in-oil emulsion, comprising (a)
a water-based phase comprising water, a cosmetically active
ingredient, and at least one coupling agent; and (b) an oil-based
phase comprising a material having a refractive index in the range
of 1.40-1.50, silicone fluids and an alkoxylated, alkyl substituted
siloxane surface active agent (e.g., dimethicone copolyol). The
composition has a refractive index in a range of 1.4026 to 1.4150.
Where the cosmetically active ingredient is an antiperspirant
active ingredient, the composition can be an antiperspirant gel
(for example, soft gel) composition. In the refractive index range
of the present invention, increased amounts of, for example,
antiperspirant active ingredient, and other high-refractive-index
materials providing cosmetic benefits, can be incorporated in the
water and oil phases of the composition while still achieving a
clear composition. The composition can also include polypropylene
glycols (for example, tripropylene glycol), as part of the
water-based phase, to provide a composition having reduced
tackiness and reduced whitening (decreased residue); this
composition is also mild.
[0013] U.S. Pat. No. 5,587,173 discloses a clear gel-type cosmetic
product which has a viscosity of at least about 50,000 centipoise
(cps) at 21.degree. C., and includes an emulsion with an oil phase
and a water phase that includes an incorporated active ingredient.
The refractive indices of the water and oil phases match to at
least 0.0004, the refractive index of the product is about 1.4000,
and the product clarity is better than thirty NTU. These formulas
contain 75-90% dispersed active phase. See also U.S. Pat. No.
4,021,536: which describes magnesium-zirconium complexes useful as
antiperspirants; and U.S. Pat. No. 5,463,098 which describes clear
antiperspirant gel stick and method for making same.
[0014] U.S. Pat. No. 3,979,510 describes aluminum-zirconium
antiperspirant systems with complex aluminum buffers, including the
use of various divalent metal ions in aluminum-zirconium
antiperspirant formulations.
[0015] U.S. Pat. No. 4,980,156 discloses improved dry-feeling
antiperspirant compositions which comprise an aqueous solution of
an astringent emulsified in a volatile silicon fluid. The emulsion
is stabilized by using a combination of a long-chain alkyl modified
polysiloxane-polyoxyalkylene copolymer and an organic surfactant
having an HLB value from 8 to 18.
[0016] U.S. Pat. No. 4,673,570 discloses uniform, clear gelled
antiperspirant compositions, free of waxes and conventional gelling
agents. The gel emulsions comprise, in combination, a volatile
silicone fluid, a silicone emulsifier, a destabilizing auxiliary
emulsifier, water, a non-volatile emollient, a coupling agent, an
active antiperspirant component and ancillary agents.
[0017] U.S. Pat. No. 5,454,026 discloses a clear antiperspirant gel
which is made by combining (a) an astringent compound having a
refractive index of 1.48 to 1.53 which is an antiperspirant salt in
the form of (i) a tray dried compound, (ii) an encapsulated salt,
or (iii) a solvent solution of a salt compound; and (b) a clear
anhydrous organic oil-free gel formed with 12-hydroxystearic acid
as the gelling agent and a blend of aromatic containing silicone
fluid and volatile silicone fluids.
[0018] U.S. Pat. No. 5,587,153 broadly discloses clear
antiperspirant gels with a refractive index of 1.3975 to 1.4025 and
a viscosity of 50,000-200,000 centipoise which are emulsions having
75-90% of a water phase.
[0019] U.S. Pat. No. 5,563,525 also discloses clear antiperspirant
gels having a viscosity of at least 50,000 centipoise and a clarity
better than 50 NTU which are emulsions having 75-90% of a water
phase.
[0020] Historically, suspension products such as sticks have
exhibited better efficacy than emulsion products. Previous attempts
have not successfully overcome the problems of improving efficacy
and achieving satisfactory formation of emulsions. Thus, it is an
object of this invention to provide improved emulsions containing
0.5-15% water which exhibit improved efficacy which efficacy is
comparable to that achieved in suspension products and, at the same
time, have a stability profile that allows for satisfactory
stability on the shelf. Another issue is the formation of emulsions
which are stable on the shelf but which destabilize sufficiently
after application to a skin surface so as to release an efficacious
amount of an active ingredient. Thus, it is an object of the
present invention to provide emulsions with those characteristics.
It is also an object of this invention to provide gel or soft solid
compositions which can, if desired, be formed into clear
compositions. It is still another object of this invention to
provide compositions that can, if desired, be formed into clear
compositions without the use of microemulsions.
SUMMARY OF THE INVENTION
[0021] This invention relates to a low water, cosmetic composition
comprising (a) 15-33% of an external phase (also called the oil
phase) which is made with at least one high refractive index (RI in
the range of 1.43-1.60) organic ester as described below; a
volatile silicone based emulsifier; and a volatile silicone; and
(b) 67-85% of an internal phase which is made with 0.5-15%,
particularly a minimum of 2% water or salt water; and at least one
active ingredient selected from the group consisting of
antiperspirant actives (particularly in a glycol solvent),
antimicrobials and fragrances, wherein (a) the refractive index of
the final cosmetic composition is in the range of 1.42-1.52 and, in
a particular embodiment, (b) the conductance of a water droplet
applied to the surface of a thin film of the cosmetic composition
is at least 250 micro Siemens/cm/ml as measured by the fixed
geometry test described below at a loading of at least 7% by weight
level of antiperspirant active as measured by a specified test
described below, with more particular embodiments having
conductances greater than 300 micro Siemens/cm/ml, particularly
greater than 400 micro Siemens/cm/ml and especially greater than
500 micro Siemens/cm/ml. The compositions of this invention are
free of borate crosslinkers.
[0022] It is important to note that while traditional gels contain
on the order of 33-50% water, the emulsions of this composition
contain 0.5-15% water.
DESCRIPTION OF THE DRAWINGS
[0023] FIG. 1 is a graphical representation of a photomicrograph as
may be obtained from an optical microscope with contrast enhanced
optics at a magnification power of 400.times. for an emulsion of
the invention as it would appear prior to application.
[0024] FIG. 2 is a graphical representation of a photomicrograph as
may be obtained from an optical microscope with contrast enhanced
optics at a magnification power of 400.times. for an emulsion of
the invention after 30 minutes on a skin surface.
[0025] A comparison between FIGS. 1 and 2 shows that the emulsion
is stable in the product container and then breaks down in use on
skin to release the active ingredient. The shaded areas represent
the external phase.
[0026] An emulsion that is representative of the type used for
generating the FIGS. 1 and 2 is described in Example 3.
DETAILED DESCRIPTION OF THE INVENTION
[0027] The low water emulsions of this invention are made by
combining 15-33% of an external phase and 67-85% of an internal
phase as described below:
[0028] External Phase (also referred to as the continuous phase)
comprising:
[0029] (a) 1-25% of an organic ester having a refractive index in
the range of 1.43-1.60 and which allows the release of an
antiperspirant active especially as marked by a specified minimum
conductance;
[0030] (b) a sufficient amount of a silicone copolyol to achieve a
solids content of 0.25-10% (particularly 0.9-4.0% and, more
particularly, 1.0-3.0%) wherein the silicone copolyol may be added
with or without solvent;
[0031] (c) a sufficient amount of a volatile silicone (for example,
a cyclomethicone such as a D5 cyclomethicone) to achieve a quantum
sufficient ("q.s.") amount of the external phase as 15-33% (for
example, wherein part of the volatile silicone may be added in a
silicone copolyol which itself is obtained already mixed with a
volatile silicone as a solvent, such as a 40-48% dimethicone
copolyol in cyclomethicone) (more particularly, 35-55% of a glycol
component for an antiperspirant product and 50-80% of a glycol
component for a deodorant product);
[0032] (d) 0-5% of a silicone elastomer (on an actives basis);
and
[0033] (e) 0-15%, particularly 0-10% and, more particularly, 0-5%
of at least one emollient;
[0034] Internal Phase (also referred to as the dispersed phase)
comprising:
[0035] (a) an effective amount of at least one cosmetically active
ingredient selected from the group consisting of 0.1-25% of an
antiperspirant active (on an anhydrous basis), 0.1-3% of a
fragrance, and 0.05-5% of an antimicrobial;
[0036] (b) a sufficient amount of a solvent component to dissolve
the cosmetically active ingredient and to complete the internal
phase (for example, a glycol component to dissolve an
antiperspirant active), with a maximum amount being about 70% of
solvent for a deodorant product and abut 80% for an antiperspirant
product;
[0037] (c) 0.5-15 % of water optionally containing up to 30 % of an
ionizable salt soluble in water (for example, NaCl, KCl,
ZnCl.sub.2, zinc citrate and zinc glycinate);
[0038] (d) 0-5 % of a non-ionic emulsifier; and
[0039] (e) 0-10% ethanol;
[0040] wherein:
[0041] (1) the final refractive index of the composition is in the
range of 1.42-1.52 (particularly 1.43-1.45);
[0042] (2) all amounts are in percent by weight based on the entire
weight of the composition; and
[0043] (3) the composition is free of borate crosslinkers.
[0044] In a particular embodiment, the conductance of a water
droplet applied to the surface of a thin film of the cosmetic
composition is at least 250 micro Siemens/cm/ml at a loading of at
least 7% by weight level of antiperspirant active as measured by
the fixed geometry test described below with more particular
embodiments having conductances greater than 300 micro
Siemens/cm/ml, particularly greater than 400 micro Siemens/cm/ml
and especially greater than 500 micro Siemens/cm/ml.
[0045] The organic esters useful in this invention include, those
of formula R"--CO(O)--R', where each of R' and R" is independently
selected from the group consisting of (a) C1-C30- straight and
branched chain alkyls and alkenyls; and (b) an aromatic group such
as phenyl, benzyl, naphthyl, or biphenyl wherein the aromatic is
optionally substituted by one or more or the groups listed in (a),
but provided that the total of the carbons for R'+R" is in the
range of 8-30.
[0046] Examples of suitable esters include, for example, C12-15
alkyl benzoate (such as FINSOLV TN from Finetex, Elmwood Park,
N.J.); octyl methoxy cinnamate (such as ESCALOL 557 from ISP,
Wayne, N.J. (but in amounts less than 6% because of irritancy);
isostearyl isostearate (such as (PRISORINE IS 2039 from Unichema,
Chicago, Ill.); benzyl benzoate; 2,6-di-(ethylhexyl)naphthalate
(such as Hallbrite TQ from the C.P. Hall Company, Bedford Park,
Ill.); butyl octyl salicylate; glyceryl monostearate; n-dibutyl
sebacate; isopropyl myristate; isopropyl palmitate; butyl stearate;
cetyl lactate; isocetyl stearate; hexyl laurate; decyl oleate;
isostearyl isostearate; ethyl hexyl maleate; sorbitan monoaurate;
sorbitan monooleate; sorbitan sesquioleate; sorbitan trioleate;
isopropyl palmitate; isopropyl stearate; stearyl stearate;
diisopropyl adipate; diisopropyl sebacate; butyl myristate; and
isopropyl laurate.
[0047] Particular esters of interest are
2,6-di-(ethylhexyl)naphthalate, octyl methoxy cinnamate; isostearyl
stearate; and C12-15 alkyl benzoate.
[0048] In general, silicone copolyols useful in the present
invention include copolyols of the following Formula I and II.
Formula I materials may be represented by:
(R.sup.10).sub.3--SiO--[(R.sup.11).sub.2--SiO].sub.x--[Si(R.sup.12)(R.sup.-
b--O--(C.sub.2H.sub.4O).sub.p--(C.sub.3H.sub.6O).sub.s--R.sup.c)O].sub.y---
Si--(R.sup.13).sub.3 Formula I
[0049] wherein each of R.sup.10, R.sup.11, R.sup.12 and R.sup.13
may be the same or different and each is selected from the group
consisting of C1-C6 alkyl; R.sup.b is the radical
--C.sub.mH.sub.2m--; R.sup.c is a terminating radical which can be
hydrogen, an alkyl group of one to six carbon atoms, an ester group
such as acyl, or an aryl group such as phenyl; m has a value of two
to eight; p and s have values such that the oxyalkylene segment
--(C.sub.2H.sub.4O).sub.p--(C.sub.3H.sub.6O).sub.s-- has a
molecular weight in the range of 200 to 5,000; the segment
preferably having fifty to one hundred mole percent of oxyethylene
units --(C.sub.2H.sub.4O).sub.p-- and one to fifty mole percent of
oxypropylene units --(C.sub.3H.sub.6O).sub.s--; x has a value of 8
to 400; and y has a value of 2 to 40. Preferably each of R.sup.10,
R.sup.11, R.sup.12 and R.sup.13 is a methyl group; R.sup.c is H; m
is preferably three or four whereby the group R.sup.b is most
preferably the radical --(CH.sub.2).sub.3--; and the values of p
and s are such as to provide a molecular weight of the oxyalkylene
segment --(C.sub.2H.sub.4O).sub.p--(C- .sub.3H.sub.6O).sub.s-- of
between about 1,000 to 3,000. Most preferably p and s should each
have a value of about 18 to 28.
[0050] A second siloxane polyether (copolyol) has the Formula
II:
(R.sup.10).sub.3--SiO--[(R.sup.11).sub.2--SiO].sub.x--[Si(R.sup.12)(R.sup.-
b--O--(C.sub.2H.sub.4O).sub.p--R.sup.c)O].sub.y----Si--(R.sup.13).sub.3
Formula II
[0051] wherein p has a value of 6 to 16; x has a value of 6 to 100;
and y has a value of 1 to 20 and the other moieties have the same
definition as defined in Formula I.
[0052] It should be understood that in both Formulas I and II shown
above, that the siloxane-oxyalkylene copolymers of the present
invention may, in alternate embodiments, take the form of
endblocked polyethers in which the linking group R.sup.b, the
oxyalkylene segments, and the terminating radical R.sup.c occupy
positions bonded to the ends of the siloxane chain, rather than
being bonded to a silicon atom in the siloxane chain. Thus, one or
more of the R.sup.10, R.sup.11, R.sup.12 and R.sup.13 substituents
which are attached to the two terminal silicon atoms at the end of
the siloxane chain can be substituted with the segment
--R.sup.b--O--(C.sub.2H.sub.4O).sub.p--(C.sub.3H.sub.6O).sub.5--R.sup.c
or with the segment --R.sup.b--O--(C.sub.2H.sub.4O).sub.p--R.sup.c.
In some instances, it may be desirable to provide the segment
--R.sup.b--O--(C.sub.2H.sub.4O).sup.p--(C.sub.3H.sub.6O).sub.s--R.sup.c
or the segment --R.sup.b--O--(C.sub.2H.sub.4O).sub.p--R.sup.c at
locations which are in the siloxane chain as well as at locations
at one or both of the siloxane chain ends.
[0053] Particular examples of suitable dimethicone copolyols are
available either commercially or experimentally from a variety of
suppliers including Dow Corning Corporation, Midland, Mich.;
General Electric Company, Waterford, N.Y.; Witco Corp., Greenwich,
Conn.; and Goldschmidt Chemical Corporation, Hopewell, Va. Examples
of specific products include DOW CORNING.RTM. 5225C from Dow
Corning which is a 10% dimethicone copolyol in cyclomethicone; DOW
CORNING.RTM. 2-5185C which is a 45-49% dimethicone copolyol in
cyclomethicone; SILWET L-7622 from Witco; ABIL EM97 from
Goldschmidt which is a 85% dimethicone copolyol in
D5cyclomethicone; and various dimethicone copolyols available
either commercially or in the literature.
[0054] It should also be noted that various concentrations of the
dimethicone copolyols in cyclomethicone can be used. While a
concentration of 10% in cyclomethicone is frequently seen
commercially, other concentrations can be made by stripping off the
cyclomethicone or adding additional cyclomethicone. The higher
concentration materials such as DOW CORNING.RTM. 2-5185 material is
of particular interest.
[0055] In one particular embodiment 0.1-40% (particularly 10-40%)
of a 10-50% silicone copolyol such as dimethicone copolyol in
cyclomethicone mixture may be used, wherein the amount of mixture
added is selected so that the level of silicone copolyol in the
cosmetic composition is in the range of 1.0-3.0% (particularly 2%)
(for example, 0.25-10% of a 40%-45% dimethicone copolyol in
cyclomethicone mixture).
[0056] By volatile silicone material is meant a material that has a
measurable vapor pressure at ambient temperature. For the volatile
silicone portion, examples of volatile silicones (particularly
silicones with a boiling point of 250 degrees C. or less at
atmospheric pressure) include cyclomethicone (especially
cyclopentasiloxane, also called "D5"), "hexamethyldisiloxane", and
low viscosity dimethicone (for example, Dow Corning.RTM. 200 fluid
having a viscosity of 1-200 centistokes). Such volatile silicones
include conventional cyclic and linear volatile silicones
Illustratively, and not by way of limitation, the volatile
silicones are one or more members selected from the group
consisting of cyclic polydimethylsiloxanes such as those
represented by Formula III: 1
[0057] where n is an integer with a value of 3-7, particularly 5-6.
For example, DC-245fluid (or the DC-345 version) from Dow Corning
Corporation (Midland, Mich.) is a type of cyclomethicone which can
be used. These include a tetramer (or
octylmethylcyclotetrasiloxane) and a pentamer (or
decamethylcyclopentasiloxane). The volatile linear silicones can
also be included in this group of volatile silicones and are one or
more members selected from the group consisting of linear
polydimethylsiloxanes such as those represented by Formula IV:
2
[0058] and t is selected to obtain a viscosity of 1-200
centistokes.
[0059] It is also possible to include a silicone elastomer in the
external phase. The elastomer may also be added in a carrier such
as cyclomethicone. Suitable elastomers include those described in,
for example, U.S. Pat. No. 6,060,546 assigned to General Electric
Company; and copending PCT case WO 99/51192, both of which are
incorporated by reference herein for the description of the
elastomers. Particular examples of suitable elastomers are SFE 167,
a cetearyl dimethicone/vinyl dimethicone crosspolymer from GE
Silicones (Waterford, N.Y.); SFE168, a cyclomethicone (and)
dimethicone/vinyl dimethicone crosspolymer from GE Silicones; vinyl
dimethicone crosspolymers such as those available from Shin Etsu
Silicones of America (Akron, Ohio) under trade names KSG-15
(cyclomethicone (and) dimethicone/vinyl dimethicone crosspolymer),
KSG-16 (dimethicone (and) dimethicone/vinyl dimethicone
crosspolymer), KSG-17 (cyclomethicone (and) dimethicone/vinyl
dimethicone crosspolymer), KSG-18 (phenyl trimethicone (and)
dimethicone/phenyl vinyl dimethicone crosspolymer); and KSG-20
(dimethicone copolyol crosspolymer; dimethicone/vinyl dimethicone
crosspolymer from Dow Corning Corporation (Midland, Mich.) under
trade name Dow Corning 9506 Cosmetic Powder; and a mixture of
cyclomethicone and stearyl-vinyl/hydromethylsiloxane copolymer
available from Grant Industries, Inc. (Elmwood Park, N.J.) under
the trade name Gransil SR-CYC.
[0060] For the antiperspirant active used in the internal (also
called "active") phase various antiperspirant active materials that
can be utilized according to the present invention provided that
they are soluble at a suitable concentration in the active phase.
These include conventional aluminum and aluminum/zirconium salts,
as well as aluminum/zirconium salts complexed with a neutral amino
acid such as glycine, as known in the art. See each of European
Patent Application Number. 512,770 A1 and PCT case WO 92/19221, the
contents of each of which are incorporated herein by reference in
their entirety, for disclosure of antiperspirant active materials.
The antiperspirant active materials disclosed therein, including
the acidic antiperspirant materials, can be incorporated in the
compositions of the present invention if they are soluble in the
active phase. Suitable materials include (but are not limited to)
aluminum chlorides (various types including, for example, anhydrous
form, hydrated form, etc.), zirconyl hydroxychlorides, zirconyl
oxychlorides, basic aluminum chlorides, basic aluminum chlorides
combined with zirconyl oxychlorides and hydroxychlorides, and
organic complexes of each of basic aluminum chlorides with or
without zirconyl oxychlorides and hydroxychlorides and mixtures of
any of the foregoing. These include, by way of example (and not of
a limiting nature), aluminum chlorohydrate, aluminum chloride,
aluminum sesquichlorohydrate, aluminum chlorohydrol-propylene
glycol complex, zirconyl hydroxychloride, aluminum-zirconium
glycine complex (for example, aluminum zirconium trichlorohydrex
gly, aluminum zirconium pentachlorohydrex gly, aluminum zirconium
tetrachlorohydrex gly and aluminum zirconium octochlorohydrex gly),
aluminum dichlorohydrate, aluminum chlorohydrex PEG, aluminum
chlorohydrex PEG, aluminum dichlorohydrex PEG, aluminum
dichlorohydrex PEG, aluminum zirconium trichlorohydrex gly
propylene glycol complex, aluminum zirconium trichlorohydrex gly
dipropylene glycol complex, aluminum zirconium tetrachlorohydrex
gly propylene glycol complex, aluminum zirconium tetrachlorohydrex
gly dipropylene glycol complex, and mixtures of any of the
foregoing. The aluminum-containing materials can be commonly
referred to as antiperspirant active aluminum salts. Generally, the
foregoing metal antiperspirant active materials are antiperspirant
active metal salts. In the embodiments which are antiperspirant
compositions according to the present invention, such compositions
need not include aluminum-containing metal salts, and can include
other antiperspirant active materials, including other
antiperspirant active metal salts. Generally, Category I active
antiperspirant ingredients listed in the Food and Drug
Administration's Monograph on antiperspirant drugs for
over-the-counter human use can be used. In addition, any new drug,
not listed in the Monograph, such as tin or titanium salts used
alone or in combination with aluminum compounds (for example,
aluminum-stannous chlorohydrates), aluminum nitratohydrate and its
combination with zirconyl hydroxychlorides and nitrates, can be
incorporated as an antiperspirant active ingredient in
antiperspirant compositions according to the present invention.
Preferred antiperspirant actives that can be incorporated in the
compositions of the present invention include the enhanced efficacy
aluminum salts and the enhanced efficacy aluminum/zirconium
salt-glycine materials, having enhanced efficacy due to improved
molecular distribution, known in the art and discussed, for
example, in PCT No. WO92/19221, the contents of which are
incorporated by reference in their entirety herein. Particular
actives include Westchlor A2Z 4105 aluminum zirconium
tetrachlorohydrex gly propylene glycol complex, (from Westwood
Chemical Corporation, Middletown, N.Y.); Westchlor ZR 35B aluminum
zirconium tetrachlorhydrex gly, and Rezal 36 GP and AZP 902
aluminum zirconium tetrachlorhydrex gly both from Reheis, Berkeley
Heights, N.J.
[0061] Antiperspirant actives can be incorporated into compositions
according to the present invention in amounts in the range of
0.05-25% (on an anhydrous solids basis), preferably 5-25%, by
weight, of the total weight of the composition. The amount used
will depend on the formulation of the composition. For example, at
amounts in the lower end of the broader range (for example,
0.05-5%), the antiperspirant active material will not substantially
reduce the flow of perspiration, but will reduce malodor, for
example, by acting as a deodorant material. At amounts at the
higher end of the range (especially using a minimum of 7% and, more
particularly, in a range of 9-20%, an antiperspirant effect can be
expected.
[0062] Deodorant active materials can be selected from several
types of materials:
[0063] (a) lesser amounts of antiperspirant actives, such as in the
range of 0.1-5.0 percent by weight based on the total weight of the
composition;
[0064] (b) fragrances, such as in the range of 0.5-3.0 percent by
weight based on the total weight of the composition;
[0065] (c) effective amounts of antimicrobial agents, for example,
0.05-5.0 percent (particularly 0.1-1% and, more particularly,
0.25-1.0%) by weight based on the total weight of the composition;
examples include bacteriostatic quaternary ammonium compounds (such
as cetyl trimethyl-ammonium bromide, and cetyl pyridinium
chloride), 2, 4, 4'-trichloro-2'-hydroxydiphenylether (Triclosan),
N-(4-chlorophenyl)-N'-(- 3,4-dichlorophenyl)urea (Triclocarban),
silver halides, octoxyglycerin (SENSIVA.TM. SC 50) and various zinc
salts (for example, zinc ricinoleate). Triclosan or Triclocarban
can, illustratively, be included in an amount of from 0.05% to
about 0.5% by weight, of the total weight of the composition.
[0066] The glycol or polyglycol is selected from the group
consisting of ethylene glycol, propylene glycol, 1,2-propanediol,
diethylene glycol, triethylene glycol, tetraethylene glycol,
dipropylene glycol, tripropylene glycol, methyl propanediol,
1,6-hexanediol, 1,3-butanediol, 1,4-butanediol, PEG-4 through
PEG-100, PPG-9 through PPG-34, pentylene glycol, neopentyl glycol,
trimethylpropanediol, 1,4-cyclohexanedimethanol- ,
2,2-dimethyl-1,3-propanediol,
2,2,4,4-tetramethyl-1,3-cyclobutanediol, and mixtures thereof. More
particular examples of the glycol component include one or more
members of the group consisting of propylene glycol, dipropylene
glycol, tripropylene glycol, 2-methyl-1,3-propanediol, methyl
propylene glycol, low molecular weight (less than 600) polyethylene
glycol, low molecular weight (less than 600) polypropylene glycols,
and mixtures of any of the foregoing. Propylene glycol is of
particular interest because the antiperspirant active is more
soluble in this type of glycol. Tripropylene glycol has lower
irritancy, but the antiperspirant active is not as soluble in this
glycol. Mixtures of glycols may be used to balance these desirable
properties.
[0067] One of the important aspects of the invention is the
presence of water in an amount of 0.5-15% (particularly 2-15%)
which optionally contains up to 30% of an ionizable salt of the
form M.sub.aX.sub.b where a=1 or 2; b=1 or 2; M is a member
selected from the group consisting of Na.sup.+1, Li.sup.+1,
K.sup.+1, Mg.sup.+2, Ca.sup.+2, Sr.sup.+2, Sn.sup.+2, and Zn
.sup.+2; and X is a member selected from the group consisting of
chloride, bromide, iodide, citrate, gluconate, lactate, glycinate,
glutamate, ascorbate, aspartate, nitrate, phosphate,
hydrogenphosphate, dihydrogenphosphate, formate, malonate, maleate,
succinate, carbonate, bicarbonate, sulfate and hydrogensulfate. A
salt of particular utility is NaCl. As will be appreciated by those
skilled in the art, while it may be possible under certain
circumstances to add a salt directly to a portion of the mixture
during manufacturing, it is preferred to add the salt as a mixture
or solution of the salt in a carrier or solvent, particularly
water. Of course, various concentration of the salt can be made
such as in the range of 1-40%, particularly 10-30% and, more
particularly, 25-30%.
[0068] It has been found that the use of water or salt water
stabilizes the emulsion which would otherwise not last more than
about 7 days at 49 degrees C. However, the amount of water used
here does not result in compositions which are so stable that they
do not release the active ingredient when the compositions are
applied to the skin. The low amount of water used in these
compositions is also important as it decreases the degradation of
the active, especially an antiperspirant salt, which is susceptible
to polymerization with a decrease in efficacy.
[0069] The stability of the emulsions of the invention may be
measured by (1) visually evaluating the emulsions for phase
separation and (2) for gels, further monitoring the rheology using
the viscosity tests described below.
[0070] The compositions of the present invention can include other
optional ingredients to improve the aesthetics and/or performance
of the cosmetic compositions of the invention. These include
colorants, fillers, fragrances, emollients, masking agents, water
soluble emollients, hydrogen bonding modifiers (for example, urea,
guanidine hydrochloride, xylitol, trehalose, maltose and
glycerine), additional fragrances, additional preservatives, etc.
Such one or more other optional ingredients can be added to the
internal or external phases or both in appropriate amounts. For
example, fragrances will frequently be partitioned to both the
external and internal phases regardless of when or to what phase
(or final product) the fragrance is added.
[0071] In a preferred embodiment the refractive indices of the
external and internal phases are matched within 0.01 to obtain a
clear product.
[0072] Emollients are a known class of materials in this art,
imparting a soothing effect to the skin. These are ingredients
which help to maintain the soft, smooth, and pliable appearance of
the skin. Emollients are also known to reduce whitening on the skin
and/or improve aesthetics. Examples of chemical classes from which
suitable emollients can be found include:
[0073] (a) fats and oils which are the glyceryl esters of fatty
acids, or triglycerides, normally found in animal and plant
tissues, including those which have been hydrogenated to reduce or
eliminate unsaturation. Also included are synthetically prepared
esters of glycerin and fatty acids. Isolated and purified fatty
acids can be esterified with glycerin to yield mono-, di-, and
triglycerides. These are relatively pure fats which differ only
slightly from the fats and oils found in nature. The general
structure may be represented by Formula VI: 3
[0074] wherein each of R.sup.1, R.sup.2, and R.sup.3 may be the
same or different and have a carbon chain length (saturated or
unsaturated) of 7 to 30. Specific examples include peanut oil,
sesame oil, avocado oil, coconut, cocoa butter, almond oil,
safflower oil, corn oil, cotton seed oil, castor oil, hydrogenated
castor oil, olive oil, jojoba oil, cod liver oil, palm oil, soybean
oil, wheat germ oil, linseed oil, and sunflower seed oil.
[0075] (b) hydrocarbons which are a group of compounds containing
only carbon and hydrogen. These are derived from petrochemicals.
Their structures can vary widely and include aliphatic, alicyclic
and aromatic compounds. Specific examples include paraffin,
petrolatum, hydrogenated polyisobutene, and mineral oil.
[0076] (c) saturated and unsaturated fatty alcohols (primary,
secondary and tertiary alcohols, and including guerbet alcohols)
with general structure: 4
[0077] wherein each of R.sup.7, R.sup.8 and R.sup.9 is hydrogen or
a straight or branched chain carbon group and the total number of
carbons in R.sup.7+R.sup.8+R.sup.9 is in the range of 7-30.
Specific examples include lauryl, myristyl, cetyl, isocetyl,
stearyl, isostearyl, oleyl, ricinoleyl and erucyl alcohol.
[0078] (d) lanolin and its derivatives which are a complex
esterified mixture of high molecular weight esters of
(hydroxylated) fatty acids with aliphatic and alicyclic alcohols
and sterols as well as propoxylated and/or butoxylated species.
Specific examples include lanolin, lanolin oil, lanolin wax,
lanolin alcohols, lanolin fatty acids, isopropyl lanolate,
propoxylated lanolin, butoxylated lanolin, and acetylated lanolin
alcohols.
[0079] (e) alkoxylated alcohols wherein the alcohol portion is
selected from aliphatic alcohols having 2-18 and more particularly
4-18 carbons, and the alkylene oxide portion is selected from the
group consisting of propylene oxide and butylene oxide having a
number of alkylene oxide units from 2-53 and, more particularly,
from 2-15. Specific examples include PPG-14 butyl ether and PPG-53
butyl ether.
[0080] (f) miscellaneous which are selected from the group
consisting of neopentyl glycol diheptanoate, PEG-8 laurate,
isocetyl stearate, dimethicone copolyol laurate, Dow Corning 2501
cosmetic wax (dimethicone copolyol); isostearyl isostearate,
isostearyl palmitate, isostearyl alcohol, PPG-5-ceteth-20,
PPG-10-cetyl ether, triethyl hexanoin, ethyl hexyl isostearate,
glyceryl oleate, and isopropyl isostearate.
[0081] (g) mixtures and blends of two or more of the foregoing.
[0082] Particular examples of suitable emollients include members
of the group consisting of Octyloxyglyderin (SENSIVA SC50 from
Schulke Mayr, Norderstedt, Germany) (which can be used as an
emollient as well as an antibacterial); Polysorbate 80 (TWEEN 80
from ICI Americas, Wilmington, Del.); Oleth-20; ethoxylated
alcohols such as steareth-2, nonoxynol-2, PPG-4-Ceteth-1;
ethoxylated carboxylic acids such as PEG-4 dilaurate, PEG-2 oleate;
glyceryl esters such as PEG-2 castor oil, polyglyceryl-3 oleate,
glyceryl stearate; sorbitan derivatives such as sorbitan oleate;
PPG-3 myristyl ether (such as WITCONOL APM from Goldschmidt), a
dimethiconol (such as Dow Corning.RTM. DC1501 dimethiconol),
neopentyl glycol diheptanoate, PEG-8 laurate, isocetyl stearate,
dimethicone copolyol laurate, Dow Corning 2501 cosmetic wax
(dimethicone copolyol); isostearyl isostearate, isostearyl
palmitate, isostearyl alcohol, PPG-5-ceteth-20, PPG-10-cetyl ether,
triethyl hexanoin, ethyl hexyl isostearate, glyceryl oleate, and
isopropyl isostearate.
[0083] The release of antiperspirant actives into the sweat is a
significant event in the development of an antiperspirant effect.
The magnitude of the antiperspirant effect is related to the
concentration of the antiperspirant salt in the sweat, and
therefore measuring the concentration of antiperspirant salt can
provide an estimate of antiperspirant efficacy. A variety of
methods can be used to evaluate antiperspirant salt concentration,
ranging from atomic absorption, ICP, and HPLC to solution
conductance of aqueous films. The later method is especially well
suited for measuring the release of small amounts of antiperspirant
salts. The methods outlined below use solution conductance to
estimate antiperspirant salt release upon short exposures to
deionized water.
[0084] As noted above, the conductance of the compositions of the
invention is defined with reference to a value of at least 250
micro Siemens/cm/ml when the composition is loaded with at least 7%
of an antiperspirant active (such as the antiperspirant actives
listed above) and when the conductance is measured by a fixed
geometry test. For purposes of clarification is should be explained
that there are a variety of tests and test conditions that can be
used to evaluate:
[0085] (1) "Conductance" is defined as an absolute measure of
current flow through a solution with the dimensions of micro
Siemens/cm, which value is independent of probe geometry. This
value is divided by the volume (in ml) of applied water to give the
conductance number with the units of micro Siemens/cm/ml. This test
is deemed a more reproducible measurement since it references a set
of fixed dimensions and units.
[0086] (2) Alternatively, "conductivity" as a measure of current
flow through a solution without reference to probe geometry, and
which is measured in micro Siemens. This test is convenient for
quick screening of solutions.
[0087] Standard Test for Thin Film Conductivity
[0088] One test for conductivity is called herein the "standard"
test. A non-conducting plastic block (for example, made from
PLEXIGLAS.RTM. material) to form an oral shaped well 12.2
cm.times.2.5 cm with a depth of 100 microns. This depth corresponds
to the mean thickness of an antiperspirant product applied to the
underarm of a human person during real use conditions
(approximately 50 to 100 microns). An aliquot of test sample is
placed in the well of the block sufficient to fill the well to the
brim. Excess sample is scraped off by running a flat edged
instrument over the surface of the block. The sample block, with
the product film, is then either (a) equilibrated at room
temperature for two hours or (b) placed in a synthetic underarm to
simulate in vivo conditions. If method (b) is used, the air
temperature inside the synthetic underarm is maintained at 33 to
35.degree. C. and a relative humidity of 85 to 95%, and the sample
blocks are placed on a temperature controlled surface maintained at
body temperature (37.degree. C.). These conditions closely
approximate the temperature gradients normally found in the
underarm. Samples are equilibrated in either the (a) or (b)
environments for two hours prior to measurement of antiperspirant
salt release by solution conductivity. After two hours the sample
blocks are removed from the controlled environment and placed on a
stage for conductivity measurement. An aliquot of 250 microliters
of water with a resistance of at least 17 mega ohms is placed on
the surface of the sample film, and the conductance of the water is
measured as a function of time with a Skicon 200 Skin surface
Hygrometer (I.B.S. Co., Ltd., Shizuoka-ken, 430, Japan) using an
Elsnau (MT-8C Probe) electrode (Todd Maibach & Associates, San
Francisco, Calif.). The electrode is positioned so that it touches
the bottom of the test sample in the well. Conductivity is measured
in micro Siemens at 3.5 MHz. Data is collected at 0.1 sec intervals
for approximately 100 sec. Solution conductivity after 10 seconds
of exposure to the water is used to compare the release of active
salt for different formulations This method is believed to be
particularly useful for evaluating the release of antiperspirant
salts in the absence of other salts. The standard method is useful
as a quick screening tool for active salt release studies. A
solution conductivity of approximately 400 or greater micro Siemens
at 10 sec after application of the water droplet to the surface of
the test sample, can be considered evidence of significant release
of the antiperspirant active salt from the film surface and
correlates with improved antiperspirant efficacy.
[0089] Fixed Geometry Test for Thin Film Conductance
[0090] One of the limitations of the Standard Test is that the area
of the water droplet is not controlled and, therefore, the apparent
conductance (which is measured as conductivity because the water
volume is not controlled) is dependent on droplet spreading. This
will lead to an underestimate of the actual solution conductance
(and therefore antiperspirant salt release), of water drops which
spread significantly. In order to measure the absolute
concentration of the antiperspirant salts the spreading of the
water drop must be stopped. This can be accomplished by placing a
well of know dimensions on the surface of the product film to
establish an area of constant size that is exposed to the water
droplet. A more predictable test is needed, such as the Fixed
Geometry Test.
[0091] The Fixed Geometry Test uses the same basic technique as the
Standard Test in terms of preparation of the test well, addition of
the test sample and equilibration of the sample to a selected
temperature. Instead of allowing the water to flow freely on the
surface of the test film, however, a second structure of
non-conducing plastic predrilled with holes of a fixed diameter is
clamped over the well block. The second structure with holes is
also made of a non-conducting material (such as PLEXIGLAS
material), is open on both ends and has an internal diameter of
1.905 cm. The bottom of each predrilled hole is fitted with a small
O-ring to prevent leakage of the water. A 400 microliter aliquot of
water (rather than the 250 microliter aliquot used in the Standard
Test) with a resistance of 17 mega Ohms is then placed in the hole
to cover the test sample. This will normally result in a liquid
height for water of about 1.4 mm. The Elsnau probe is positioned
through the drilled hole so that the bottom of the probe rests on
the bottom of the well at a right angle. Because of the fixed
shape, data can be obtained as conductance in micro Siemens/cm/ml
using the method described for calculation.
[0092] As will be appreciated by those skilled in the art, a
variety of other shapes, sizes and orientations of electrodes can
be used. In another variation on the Fixed Geometry Test, thin gold
wires (99% purity, set of 2, each about 1 mm in diameter) can be
constructed to be in parallel with the surface of the water (and
covered by the water) and conductance can be measured.
[0093] The electrode used in both types of tests must be calibrated
so that a conductivity in micro Siemens can be obtained. Such
calibration with a salt solutions in water of known conductance is
known to those skilled in the art.
[0094] While different readings can be obtained depending on the
thickness of the films, the test used, etc. it is important to
establish a standard test for purposes of defining conductivity
according to this invention. The Fixed Geometry Test is set as the
defining test because it is believed to be more reproducible. Thus
a minimum conductance value of 250 micro Siemens/cm/ml is the lower
limit. Interestingly, minimum values for the Standard Test seemed
to run about 400 micro Siemens due to the way the test was
conducted. For the data described here, samples should be placed in
a chamber at the humidity and elevated temperature conditions
described above for about 2 hours. Samples not subjected to
elevated temperatures should give higher values.
[0095] An average efficacy gel having a water content of greater
than 35% (such as Gillette's Right Guard Antiperspirant Gel) was
compared with an improved gel made according to Example 3, below.
The average efficacy gel has a standard conductivity of 295.+-.35
micro Siemens at 10seconds and a fixed geometry conductivity of
121.+-.47 micro Siemens/cm/ml at 10seconds. The improved
formulation made according to this invention had a standard
conductivity of 1884.+-.225 micro Siemens at 10seconds and a fixed
geometry conductance of 1213.+-.43 micro Siemens/cm/ml at
10seconds. The improved formulation was ranked as above average in
efficacy in a clinical test whereas the average gel was ranked as
average in efficacy in a clinical test.
[0096] While it is not known precisely how the compositions of this
invention work, it has been observed that they have a combination
of two important properties. These compositions exhibit superior
stability on the shelf and yet degrade on contact with the skin to
release the active ingredient with a higher level of efficacy than
is usually achieved. The deodorant and/or antiperspirant
compositions disclosed in this invention form metastable emulsions
when deposited on the skin. The decomposition of these emulsions
upon application can be assessed by the thin film conductance
method described herein. In another test the superiority of this
invention is evaluated by applying test sample on skin, waiting 30
minutes, gently scraping the sample off the skin, placing the
scraped emulsion on a slide with a cover and examining the product
film under a microscope with contrast enhanced optics. Comparison
to another experimental low efficacy formulations containing an
antiperspirant active shows that the emulsions of effective
formulations break up on the skin while the emulsions of the low
efficacy samples remain intact. (See FIGS. 1 and 2 above.)
[0097] Particular formulations of interest include:
[0098] Formulation A:
[0099] External Phase comprising:
[0100] (a) 0.5-25% (particularly 5-15%) of C12-15 alkyl
benzoate;
[0101] (b) 0.1-7% (particularly 2-5%) of a 40% dimethicone copolyol
in cyclomethicone);
[0102] (c) 0-25% (particularly 5-15%) of a volatile silicone (for
example, a cyclomethicone such as a D5 cyclomethicone);
[0103] (d) 0-5% (particularly 0.1-2%) of a silicone elastomer
(actives basis) (cyclomethicone carrier);
[0104] Internal Phase comprising:
[0105] (a) 0.1-25% of an antiperspirant active (on an anhydrous
basis) (especially 7-25% for an antiperspirant or 0.1-5% for a
deodorant);
[0106] (b) a sufficient amount of a glycol component such as
propylene glycol to dissolve the antiperspirant active and to
complete the internal phase;
[0107] (c) 0.5-15% (particularly 2-5%) water;
[0108] (d) 0-5% nonionic emulsifier (for example, Oleth-20);
[0109] (e) 0-3% NaCl (0-3% on a dry basis but added in a 20-30%
water solution).
[0110] Formulation B:
[0111] External Phase comprising:
[0112] (a) 0.5-25% of octyl methoxy cinnamate;
[0113] (b) 0.1-7% (particularly 2-5%) of a 40% dimethicone copolyol
in cyclomethicone);
[0114] (c) 0-25% (particularly 5-15%) of a volatile silicone, (for
example, a cyclomethicone such as a D5 cyclomethicone);
[0115] (d) 0-5% (particularly 0.1-2%) of a silicone elastomer
(actives basis) (cyclomethicone carrier);
[0116] Internal Phase comprising:
[0117] (a) 0.1-25% of an antiperspirant active (on an anhydrous
basis) (especially 7-25% for an antiperspirant or 0.1-5% for a
deodorant);
[0118] (b) a sufficient amount of a glycol component such as
propylene glycol to dissolve the antiperspirant active and to
complete the internal phase;
[0119] (c) 0.5-15% (particularly 2-15%) water;
[0120] (d) 0-5% nonionic emulsifier (for example, Oleth-20);
[0121] (e) 0-3% NaCl (0-3% on a dry basis but added in a 20-30%
water solution).
[0122] Formulation C:
[0123] External Phase comprising:
[0124] (a) 0.5-25% of isostearyl isostearate;
[0125] (b) 0.1-7% (particularly 2-5%) of a 40% dimethicone copolyol
in cyclomethicone);
[0126] (c) 0-25% (particularly 5-15%) of a volatile silicone, (for
example, a cyclomethicone such as a D5 cyclomethicone);
[0127] (d) 0-5% (particularly 0.1-2%) of a silicone elastomer
(actives basis) (cyclomethicone carrier);
[0128] Internal Phase comprising:
[0129] (a) 0.1-25% of an antiperspirant active (on an anhydrous
basis) (especially 7-25% for an antiperspirant or 0.1-5% for a
deodorant);
[0130] (b) a sufficient amount of a glycol component such as
propylene glycol to dissolve the antiperspirant active and to
complete the internal phase;
[0131] (c) 0.5-15% (particularly 2-15%) water;
[0132] (d) 0-5% nonionic emulsifier (for example, Oleth-20);
[0133] (e) 0-3% NaCl (0-3% on a dry basis but added in a 20-30%
water solution).
[0134] Formulation D:
[0135] External Phase comprising:
[0136] (a) 0.5-25% of benzyl benzoate;
[0137] (b) 0.1-7% (particularly 2-5%) of a 40% dimethicone copolyol
in cyclomethicone);
[0138] (c) 0-25% (particularly 5-15%) of a volatile silicone, (for
example, a cyclomethicone such as a D5 cyclomethicone);
[0139] (d) 0-5% (particularly 0.1-2%) of a silicone elastomer
(actives basis) (cyclomethicone carrier);
[0140] Internal Phase comprising:
[0141] (a) 0.1-25% of an antiperspirant active (on an anhydrous
basis) (especially 7-25% for an antiperspirant or 0.1-5% for a
deodorant);
[0142] (b) a sufficient amount of a glycol component such as
propylene glycol to dissolve the antiperspirant active and to
complete the internal phase;
[0143] (c) 0.5-15% (particularly 2-15%) water;
[0144] (d) 0-5% nonionic emulsifier (for example, Oleth-20);
[0145] (e) 0-3% NaCl (0-3% on a dry basis but added in a 20-30%
water solution).
[0146] Formulation E:
[0147] External Phase comprising:
[0148] (a) 0.5-25% (particularly 1-10% of a combination of 2,6
diethylhexylnaphthalate, isostearyl stearate and C12-15 alkyl
benzoate wherein the mixture of esters has a refractive index in
the range of 1.45-1.54;
[0149] (b) 0.1-7% (particularly 2-5%) of a 40% dimethicone copolyol
in cyclomethicone);
[0150] (c) 0-25% (particularly 5-15%) of a volatile silicone, (for
example, a cyclomethicone such as a D5 cyclomethicone);
[0151] (d) 0-5% (particularly 0.1-2%) of a silicone elastomer
(actives basis) (cyclomethicone carrier);
[0152] Internal Phase comprising:
[0153] (a) 0.1-25% of an antiperspirant active (on an anhydrous
basis) (especially 7-25% for an antiperspirant or 0.1-5% for a
deodorant);
[0154] (b) a sufficient amount of a glycol component such as
propylene glycol to dissolve the antiperspirant active and to
complete the internal phase;
[0155] (c) 0.5-15% (particularly 2-15%) water;
[0156] (d) 0-5% nonionic emulsifier (for example, Oleth-20);
[0157] (e) 0-3% NaCl (0-3% on a dry basis but added in a 20-30%
water solution).
[0158] Formulation F: Same as Formulation E but with the ester
component being made with 0.5-14.5% (particularly 2-10%) C12-15
alkyl benzoate and 0.5-14.5% (particularly 2-10%) isostearyl
stearate.
[0159] Formulation G: Same as Formulation E but with the ester
component being made with 0.5-14.5% (particularly 2-10%) C12-15
alkyl benzoate and 0.5-14.5% (particularly 2-10%) 2,6
diethylhexylnaphthalate.
[0160] Formulation H: Same as Formulation E but with the ester
component being made with 0.5-14.4% (particularly 5-10%) C12-15
alkyl benzoate; and 0.5-14.4% (particularly 5-10%) benzyl benzoate;
and 1-5% (particularly 0.1-4%) octyl methoxy cinnamate.
[0161] Formulae I-P
[0162] Any of Formulae A-H where a water soluble salt, an aqueous
solution of a water soluble salt or and ethanol/water solution of a
water soluble salt is used instead of water. Examples with NaCl
have been listed above, but specific salts also include ZnCl.sub.2,
zinc citrate, zinc gluconate magnesium sulfate, strontium lactate,
sodium acetate, zinc acetate, and calcium chloride, particularly
when the salt is added as a premixture of 10-30%, especially
25-30%, solution made with water, ethanol or a water/ethanol
mixture.
[0163] Formulation I:
[0164] External Phase: Same as Formulation A.
[0165] Internal Phase comprising:
[0166] (a) 0.1-25% of an antiperspirant active (on an anhydrous
basis) (especially 7-25% for an antiperspirant or 0.1-5% for a
deodorant);
[0167] (b) a sufficient amount of a glycol component such as
propylene glycol to dissolve the antiperspirant active and to
complete the internal phase;
[0168] (c) 0.5-15% (particularly 2-5%) water;
[0169] (d) 0-5% nonionic emulsifier (for example, Oleth-20);
[0170] (e) 0-15% of a 30% ZnCl.sub.2 water solution.
[0171] Formulation J:
[0172] External Phase Same as Formulation B.
[0173] Internal Phase comprising:
[0174] (a) 0.1-25% of an antiperspirant active (on an anhydrous
basis) (especially 7-25% for an antiperspirant or 0.1-5% for a
deodorant);
[0175] (b) a sufficient amount of a glycol component such as
propylene glycol to dissolve the antiperspirant active;
[0176] (c) 0.5-15% (particularly 2-5%) water;
[0177] (d) 0-5% nonionic emulsifier (for example, Oleth-20);
[0178] (e) 0-15% of a 10% zinc gluconate water solution.
[0179] Formulation K:
[0180] External Phase Same as Formulation C.
[0181] Internal Phase comprising:
[0182] (a) 0.1-25% of an antiperspirant active (on an anhydrous
basis) (especially 7-25% for an antiperspirant or 0.1-5% for a
deodorant);
[0183] (b) a sufficient amount of a glycol component such as
propylene glycol to dissolve the antiperspirant active and to
complete the internal phase;
[0184] (c) 0.5-15% (particularly 2-5%) water;
[0185] (d) 0-5% nonionic emulsifier (for example, Oleth-20);
[0186] (e) 0-9% of a 30% ZnCl.sub.2 ethanolic solution.
[0187] Formulation L:
[0188] External Phase Same as Formulation D.
[0189] Internal Phase comprising:
[0190] (a) 0.1-25% of an antiperspirant active (on an anhydrous
basis) (especially 7-25% for an antiperspirant or 0.1-5% for a
deodorant);
[0191] (b) a sufficient amount of a glycol component such as
propylene glycol to dissolve the antiperspirant active and to
complete the internal phase;
[0192] (c) 0.5-15% (particularly 2-5%) water;
[0193] (d) 0-5% nonionic emulsifier (for example, Oleth-20);
[0194] (e) 0-9% of a 25% strontium lactate aqueous solution.
[0195] Formulation M:
[0196] External Phase Same as Formulation E.
[0197] Internal Phase comprising:
[0198] (a) 0.1-25% of an antiperspirant active (on an anhydrous
basis) (especially 7-25% for an antiperspirant or 0.1-5% for a
deodorant);
[0199] (b) a sufficient amount of a glycol component such as
propylene glycol to dissolve the antiperspirant active and to
complete the internal phase;
[0200] (c) 0.5-15% (particularly 2-5%) water;
[0201] (d) 0-5% nonionic emulsifier (for example, Oleth-20);
[0202] (e) 0-9% of a magnesium sulfate solution.
[0203] Formulation N:
[0204] External Phase Same as Formulation F.
[0205] Internal Phase comprising:
[0206] (a) 0.1-25% of an antiperspirant active (on an anhydrous
basis) (especially 7-25% for an antiperspirant or 0.1-5% for a
deodorant);
[0207] (b) a sufficient amount of a glycol component such as
propylene glycol to dissolve the antiperspirant active and to
complete the internal phase;
[0208] (c) 0.5-15% (particularly 2-5%) water;
[0209] (d) 0-5% nonionic emulsifier (for example, Oleth-20);
[0210] (e) 0-9% of a sodium acetate aqueous solution.
[0211] Formulation O:
[0212] External Phase Same as Formulation G.
[0213] Internal Phase comprising:
[0214] (a) 0.1-25% of an antiperspirant active (on an anhydrous
basis) (especially 7-25% for an antiperspirant or 0.1-5% for a
deodorant);
[0215] (b) a sufficient amount of a glycol component such as
propylene glycol to dissolve the antiperspirant active and to
complete the internal phase;
[0216] (c) 0.5-15% (particularly 2-5%) water;
[0217] (d) 0-5% nonionic emulsifier (for example, Oleth-20);
[0218] (e) 0-9% of a zinc acetate 10% aqueous solution.
[0219] Formulation P:
[0220] External Phase Same as Formulation H
[0221] Internal Phase comprising:
[0222] (a) 0.1-25% of an antiperspirant active (on an anhydrous
basis) (especially 7-25% for an antiperspirant or 0.1-5% for a
deodorant);
[0223] (b) a sufficient amount of a glycol component such as
propylene glycol to dissolve the antiperspirant active and to
complete the internal phase;
[0224] (c) 0.5-15% (particularly 2-5%) water;
[0225] (d) 0-5% nonionic emulsifier (for example, Oleth-20);
[0226] (e) 0-9% of a 30% calcium chloride aqueous solution.
[0227] Formulations Q-X:
[0228] Any of Formulae A-H where the composition comprises an
additional ingredient of up to 10% ethanol which is substituted for
a portion of the water content.
[0229] Formulation Y:
[0230] External Phase comprising:
[0231] (a) 0.5-25% (particularly 5-15%) of C12-15 alkyl
benzoate;
[0232] (b) 0.1-7% (particularly 3.0-6.0) of a 48% dimethicone
copolyol in cyclomethicone) (or an equivalent amount of actives if
other concentrations are used);
[0233] (c) 0-25% (particularly 5-15%) of a volatile silicone (for
example, a cyclomethicone such as a D5 cyclomethicone);
[0234] (d) 0-5% (particularly 0.1-2%) of a silicone elastomer
(actives basis) (cyclomethicone carrier);
[0235] Internal Phase comprising:
[0236] (a) 0.1-25% of an antiperspirant active (on an anhydrous
basis) (especially 7-25% for an antiperspirant or 0.1-5% for a
deodorant);
[0237] (b) a sufficient amount of a glycol component such as
propylene glycol to dissolve the antiperspirant active (for
example, 35-55% of a glycol component for an antiperspirant product
and 50-80% of a glycol component for a deodorant product);
[0238] (c) 0.5-15% (particularly 2-5%) water;
[0239] (d) 0-5% nonionic emulsifier (for example, Oleth-20);
[0240] (e) 0-3% NaCl (0-3% on a dry basis but added in a 20-30%
water solution);
[0241] and
[0242] (f) 0-12% alcohol (for example, 5-15% of 95% ethanol).
[0243] Formulation Z:
[0244] External Phase comprising:
[0245] (a) 0.5-25% (particularly 5-15%) of C12-15 alkyl
benzoate;
[0246] (b) 0.1-7% (particularly 6-12%) of a 25% dimethicone
copolyol in cyclomethicone);
[0247] (c) 0-25% (particularly 5-15%) of a volatile silicone (for
example, a cyclomethicone such as a D5 cyclomethicone);
[0248] (d) 0-5% (particularly 0.1-2%) of a silicone elastomer
(actives basis) (cyclomethicone carrier);
[0249] Internal Phase comprising:
[0250] (a) 0.1-25% of an antiperspirant active (on an anhydrous
basis) (especially 7-25% for an antiperspirant or 0.1-5% for a
deodorant);
[0251] (b) a sufficient amount of a glycol component such as
propylene glycol to dissolve the antiperspirant active and to
complete the internal phase;
[0252] (c) 0.5-15% (particularly 2-5%) water;
[0253] (d) 0-5% nonionic emulsifier (for example, Oleth-20);
[0254] (e) 0-3% NaCl (0-3% on a dry basis but added in a 20-30%
water solution).
[0255] Formulation AA:
[0256] External Phase: Same as Formulation A
[0257] Internal Phase:
[0258] (a) 0.05-5.0% of an antibacterial agent
[0259] (b)-(e) same as Formulation A.
[0260] Formulation BB:
[0261] External Phase: Same as Formulation B
[0262] Internal Phase:
[0263] (a) 0.05-5.0% of an antibacterial agent
[0264] (b)-(e) same as Formulation B.
[0265] Formulation CC:
[0266] External Phase: Same as Formulation C
[0267] Internal Phase:
[0268] (b) 0.05-5.0% of an Antibacterial
[0269] (b)-(e) same as Formulation C.
[0270] Formulation DD:
[0271] External Phase: Same as formulation D
[0272] Internal Phase:
[0273] a) 0.05-5.0% of an antibacterial agent
[0274] (b)-(e) same as Formulation D.
[0275] While the mechanism of how this invention provides improved
efficacy is not completely understood, it is believed that the
invention solves two problems. The first problem is the barrier
problem which is caused, in significant part, by the presence of a
non-volatile silicone component. The second problem is the
stability of the emulsion which, if too stable, results in failure
of the antiperspirant to be released after application to the skin
and a reduction in efficacy. This invention overcomes both of these
problems with (a) the significant reduction (particularly not to
exceed a level of 5% by weight) or, preferably, total elimination
of the non-volatile silicone components that are frequently used in
antiperspirant and/or deodorant products and (b) the creation of
emulsion that exhibit satisfactory stability on the shelf and yet
break down when applied to the skin to release the antiperspirant
active allow for improved performance. As an additional benefit,
the formulations of this invention may be made as clear products
without the use of microemulsions.
[0276] The cosmetic composition according to the present invention
can be packaged in conventional containers, using conventional
techniques. Where a gel, cream or soft-solid cosmetic composition
is produced, the composition can be introduced into a dispensing
package (for example, conventional packages for gels with glide on
applicators, jars where the gel or cream is applied by hand, and
newer style packages having a top surface with pores) as
conventionally done in the art. Thereafter, the product can be
dispensed from the dispensing package as conventionally done in the
art, to deposit the active material, for example, on the skin. For
roll-ons the compositions can be placed in a conventional type of
container. This provides good deposition of the active material on
the skin.
[0277] Compositions of the present invention can be formulated as
clear, translucent or opaque products, although clear products are
preferred. A desired feature of the present invention is that a
clear, or transparent, cosmetic composition, (for example, a clear
or transparent deodorant or antiperspirant composition) can be
provided. The term clear or transparent according to the present
invention is intended to connote its usual dictionary definition;
thus, a clear liquid or gel antiperspirant composition of the
present invention allows ready viewing of objects behind it. By
contrast, a translucent composition, although allowing light to
pass through, causes the light to be scattered so that it will be
impossible to see clearly objects behind the translucent
composition. An opaque composition does not allow light to pass
therethrough. Within the context of the present invention, a gel or
stick is deemed to be transparent or clear if the maximum
transmittance of light of any wavelength in the range 400-800 nm
through a sample 1 cm thick is at least 35%, preferably at least
50%. The gel or liquid is deemed translucent if the maximum
transmittance of such light through the sample is between 2% and
less than 35%. A gel or liquid is deemed opaque if the maximum
transmittance of light is less than 2%. The transmittance can be
measured by placing a sample of the aforementioned thickness into a
light beam of a spectrophotometer whose working range includes the
visible spectrum, such as a Bausch & Lomb Spectronic 88
Spectrophotometer. As to this definition of clear, see European
Patent Application Publication No. 291,334 A2. Thus, according to
the present invention, there are differences between transparent
(clear), translucent and opaque compositions.
[0278] Compositions of the present invention may be made by the
techniques described in the Examples below. In general, the
external and internal phases are formed separately using heating
with the addition of a non-ionic emulsifier as needed. The alcohol
component is added to the internal phase. The internal phase is
added to the external phase very slowly. After the addition has
been completed, the mixture is stirred at speeds on the order of
500-1000 rpm (for example, 1000 rpm), to achieve a homogeneous
mixture, followed by homogenization at speeds which are correlated
with a voltage setting of about 55-65, particularly 60, on a
Powerstat Variable Autotransformer to achieve the target viscosity.
Compositions with a viscosity of 0-50,000 centipoise, especially
5,000-20,000 centipoise, may be suitable for roll-on products while
compositions having a viscosity on the order of 50-400,000
centipoise may be more suitable for soft solids or creams.
[0279] A variety of equipment and techniques may be used to obtain
the compositions of the invention, including one pass
homogenization, colloidal mill. Examples of such equipment include
Sonic Production Sonolator 200-30, and Sonic Tri-Homo Colloid Mill
both of which may be obtained from Sonic Corporation, Stratford,
Conn.
[0280] It is believed that the more homogeneous the composition is
and the more uniform the particle size, the better properties of
the composition.
[0281] Throughout the present specification, where compositions are
described as including or comprising specific components or
materials, or where methods are described as including or
comprising specific steps, it is contemplated by the inventors that
the compositions of the present invention also consist essentially
of, or consist of, the recited components or materials, and also
consist essentially of, or consist of, the recited steps.
Accordingly, throughout the present disclosure any described
composition of the present invention can consist essentially of, or
consist of, the recited components or materials, and any described
method of the present invention can consist essentially of, or
consist of, the recited steps.
EXAMPLES
[0282] The following Examples are offered as illustrative of the
invention and are not to be construed as limitations thereon. In
the Examples and elsewhere in the description of the invention,
chemical symbols and terminology have their usual and customary
meanings. In the Examples as elsewhere in this application values
for n, m, etc. in formulas, molecular weights and degree of
ethoxylation or propoxylation are averages. Temperatures are in
degrees C. unless otherwise indicated. The alcohol used was 95%
unless otherwise indicated. Unless otherwise indicated, "water" or
"D.I. water" mean deionized water. As is true throughout the
application, the amounts of the components are in weight percents
based on the standard described; if no other standard is described
then the total weight of the composition is to be inferred. Various
names of chemical components include those listed in the CTFA
International Cosmetic Ingredient Dictionary (Cosmetics, Toiletry
and Fragrance Association, Inc., 7.sup.th ed. 1997). Viscosities
are measured using Brookfield viscometers unless otherwise
indicated. While specific amounts of particular elastomers have
been described, there are chemical differences in the variety of
elastomers that are available. The use of different elastomers may
result in the need to increase or decrease the amount of elastomer
used in a particular formulation, especially if a clear product is
desired.
Example 1
General Method--No Elastomer
[0283] In general, the external and internal phases are formed
separately either at room temperature or with heating as described
below. The internal phase is added to the external phase very
slowly while stirring at to form an emulsion. After the addition
has been completed, the mixture is stirred at higher speed to
achieve a homogeneous mixture. The final formula viscosity is then
achieved by homogenizing the emulsion under either batch or
continuous process conditions as described below. The fragrance may
be added at any time during the process prior to final
homogenization.
[0284] Preparation of External Phase:
[0285] The ingredients to be used in the external phase are weighed
out at room temperature and combined in a suitable vessel such as a
2 liter glass beaker. The mixture is stirred at about 500 rpm for
15-20 minutes using an overhead mixer such as a Lightnin Mixer
Model L1003. If a waxy or solid emollient is to be added to the
external (also called "continuous") phase, the mixture may be
heated to facilitate dissolution while stirring then cooled to room
temperature prior to combination with the internal phase as
described below.
[0286] Preparation of Internal Phase:
[0287] The internal dispersed phase is prepared as described below.
Ingredients are mixed for a time sufficient to achieve homogeneity.
The antiperspirant active used (for example, Westchlor A2Z4105 (28%
aluminum-zirconium glycinate in propylene glycol)) is weighed into
a large beaker equipped with an overhead stirrer. Other internal
phase ingredients are then added while stirring.
[0288] The fragrance (if any is used) is added last and may be
added either to the internal phase or the external phase or the
final formula prior to homogenization. For many of the examples
described here, one could add the fragrance to the internal
phase.
[0289] If an optional non-ionic emulsifier such as Oleath-20is
used, the emulsifier and propylene glycol are combined in a
separate beaker and heated to 40 degrees C. with stirring until the
non-ionic emulsifier completely dissolved. The heat is turned off
and the remaining ingredients to be used in the internal phase,
including the antiperspirant active are weighed out and added to
the mixture of propylene glycol and non-ionic emulsifier.
[0290] If water or a salt solution are used, the internal phase is
prepared as follows. The solution containing antiperspirant active
salt as received from supplier is weighed into a large beaker
equipped with a magnetic stirrer. Additional ingredients such as
propylene glycol, ethanol and water are added while stirring. If a
salt water solution is used (such as for NaCl, etc.), the salt
water solution is prepared by dissolving the crystalline salt in
water in a separate beaker and stirring until dissolved. The salt
water solution is then added to the rest of the internal phase and
the mixture is stirred until homogeneous.
[0291] Preparation of the Emulsion:
[0292] The internal phase made as described above is then added to
the external phase over the course of 15-30 minutes while stirring
at a speed of 500-1000 RPM. After the addition is complete, the
mixture is stirred at 1000-1300 rpm for 20 minutes using a Lightnin
Mixer Model L1003. The mixture is then homogenized for 2-4 minutes
using a homogenizer from Greerco Corp., Hudson, N.H. at a reading
of about 60 on a Powerstat Variable Autotransformer from Superior
Electric Co., Bristol, Conn.
[0293] Further Processing:
[0294] The product is then further processed by homogenized to
achieve the desired final viscosity. This can be done by using a
Gilford-Wood Model 1-L (Greerco Corp., Hudson, N.H.) homogenizer.
The homogenizer speed is controlled by a Powerstat Variable
Autotransformer Type 3PN116B (Superior Electronic. Co., Bristol,
Conn.). Typical voltage setting and processing time are chosen to
give a desired final formula viscosity.
[0295] An other method of homogenization of the final product is to
pass the emulsion through a colloid mill such as a Sonic Tri-Homo
Colloid Mill or a process sonolator such Sonic Production Sonolator
200-30 both available from Sonic Corporation of Stratford, Conn.
Process conditions are chosen to give the desired final product
viscosity.
Example 1B
Evaluation of Viscosity
[0296] Brookfield Viscosity
[0297] Viscosity can be measured using a Brookfield instrument
(Model DV11+) with an E Spindle at 2.5 revolutions per minute (rpm)
and a setting of S 95. Units are in centipoise ("cps").
[0298] Carri-Med Viscosity
[0299] A second way of evaluating rheology is with the use of
Carri-Med equipment to obtain complex viscosity. Rheological
parameters can be measured using a Carri-Med CSL 100 instrument
with parallel plates. Initially the zero gap is set on the
instrument. A sample of approximately 5 grams is placed on the
stage of the instrument. A 15 minute compression is used for sample
equilibration. The excess of the sample is scraped around the plate
geometry. The rheological parameters G, G", tan (delta) and complex
viscosity (n*) can be measured by torque sweep experiments. An
acrylic plate 6 cm in diameter can be used. A gap (1000 microns) is
used between the two plates. Temperature is maintained at 23
degrees C. The oscillation stress can be varied from 2.358 Pa to
50.74 Pa with an oscillation frequency kept constant at 1 Hertz.
Units are in Pascal seconds ("Pa sec").
Example 2
General Method With Elastomer
[0300] The Method of Example 1 can be repeated with the addition of
an elastomer component. The elastomer component is obtained as a
suspension of elastomer in cyclomethicone (for example at a
concentration of 5.8% active in D5 cyclomethicone). The elastomer
component is added to the external phase with stirring at high
speed (800-1000 rpm for a 1 kilogram batch) until no particles of
elastomer are visible to the eye.
Examples 3-6
[0301] The method of Example 1 is repeated with the types and
amounts of ingredients listed in Table I. Viscosity measurements
can be obtained using the methods described in Example 1 to obtain
the data as listed in Table I.
1TABLE I Ingredient Ex. 3 Ex. 4 Ex. 5 Ex. 6 Ex. 7 Cyclomethicone
3.75 3.75 6.0 6.0 3.75 and dimethicone copolyol (48%) DC 2-5185C
Cyclomethicone 9.75 7.75 11.1 11.8 9.75 (D5) C12-15 alkyl 10.5 10.5
13.7 13.7 10.5 benzoate Dimethiconol.sup.a 0 2.0 0 0 0 Al-Zr gly in
54.0 54.0 53.75 53.75 54.0 propylene glycol (28%) Propylene glycol
8.0 8.0 0 1.3 8.0 SD Alcohol 40 9.0 9.0 0 0 0 (95%) Water* 4.0 4.0
12.13 12.13 11.0 NaCl.sup.b 0 0 2.0 0 0 Fragrance 1.0 1.0 1.0 1.0
1.0 Oleth-20 0 0 0.5 0.5 0 Urea 0 0 0 0 2.0 Initial complex 200-220
200-220 200-220 120-135 n.d. viscosity.sup.c (Pa Sec) Complex
200-220 200-220 155-170 70-80 n.d. Viscosity.sup.c (after 4 weeks @
49.degree. C.) (Pa sec) Conductivity.sup.d 1884 1985 >1000 n.d.
n.d. .sup.a = Silicone DC 1501 Fluid (long chain polysiloxane).
.sup.b = NaCl and water are premixed and added together. .sup.c =
CarriMed technique to be used for complex viscosities. .sup.d =
Standard Test as described above with units in micro Siemens.
Examples 8-11
[0302] The method of Example 1 may be repeated with the types and
amounts of ingredients listed in Table II. Viscosity measurements
can be obtained using the methods described in Example 1 to obtain
the data as listed in Table II.
2TABLE II Ingredient Ex. 8 Ex. 9 Ex. 10 Ex. 11 Cyclomethicone and
dimethicone 5.15 5.15 5.06 5.06 copolyol (48%) DC 2185C
Cyclomethicone (D5) 8.75 8.75 8.01 8.01 C12-15 alkyl benzoate 11.1
11.1 11.29 11.12 Al-Zr gly in propylene glycol (28%) 59.57 59.57
58.13 58.13 Propylene glycol 0 0 0 2.21 SD Alcohol 40 (95%) 0 0 0 0
Water* 11.93 12.43 13.16 13.16 NaCl.sup.a 2.0 2.0 2.0 0 Fragrance
1.0 1.0 1.0 1.0 Oleth-20 0.5 0 0.54 0.5 Dimethicone (100
centistokes) 0 0 0.81 0.81 Initial complex viscosity.sup.b (Pa sec)
n.d. n.d 200- 105- 215 115 Conductivity.sup.c n.d. n.d. n.d. 1623
.sup.a = NaCl and water are premixed and added together. .sup.b =
CarriMed technique to be used for complex viscosities. .sup.c =
Standard Test as described above with units in micro Siemens.
Examples 16-19
[0303] The method of Example 1 may be repeated with the types and
amounts of ingredients listed in Table III. Viscosity measurements
can be obtained using the methods described in Example 1 to obtain
the data as listed in Table III.
3TABLE III Ingredient Ex. 16 Ex. 17 Ex. 18 Ex. 19 Cyclomethicone
and dimethicone 3.75 3.75 3.75 6.0 copolyol (48%) DC 2185C
Cyclomethicone (D5) 10.25 10.25 9.25 11.1 C12-15 alkyl benzoate 0
5.0 0 13.7 Benzyl benzo ate 10.0 5.0 0 0 Isostearyl isostearate 0 0
11.0 0 Al-Zr gly in propylene glycol 54.0 54.0 54.0 53.57 (28%)
Propylene glycol 8.0 8.0 8.0 0 SD Alcohol 40 (95%) 9.0 9.0 9.0 0
Water.sup.a 4.0 4.0 4.0 11.13 ZnCl.sub.2.sup.a 0 0 0 3.0 Fragrance
1.0 1.0 1.0 1.0 Oleth-20 0 0 0 0.5 .sup.a = ZnCl.sub.2 and water
are premixed and added together.
Examples 20-23
[0304] The method of Example 1 may be repeated with the types and
amounts of ingredients listed in Table IV. Viscosity measurements
can be obtained using the methods described in Example 1 to obtain
the data as listed in Table IV.
4TABLE IV Ingredient Ex. 20 Ex. 21 Ex. 22 Ex. 23 Cyclomethicone and
dimethicone 6.0 6.0 5.0 5.5 copolyol (48%) Cyclomethicone (D5) 9.1
9.1 8.8 9.1 C12-15 alkyl benzoate 11.4 10.4 10.2 10.4 Al-Zr gly in
propylene glycol 58.07 57.57 53.57 58.57 (28%) Propylene glycol
3.93 0.5 0.43 4.43 SD Alcohol 40 (95%) with 0 9.0 with ZnCl.sub.2
ZnCl.sub.2 Water 0 with with 0 ZnCl.sub.2 ZnCl.sub.2 ZnCl.sub.2
(20% in water) 0 14.93 12.0 0 ZnCl.sub.2 (18.1% in 95% ethanol)
11.0 0 0 11.0 Fragrance 1.0 1.0 1.0 1.0 Oleth-20 0.5 0.5 0 0
Example 24-27
[0305] The method of Example 1 may be repeated with the following
amounts of ingredients listed in Table V may be used to make
compositions according to the invention.
5TABLE V Ingedient Ex. 24 Ex. 26 Ex. 27 Ex. 25A Ex. 25B Ex. 25C
Cyclomethicone and 5.00 4.06 4.15 5.25-5.75 5.25-5.75 5.25-5.75
dimethicone copolyol (40%) Cyclomethicone (D5) 12.1 9.01 9.75
8.25-8.75 8.25-8.75 8.25-8.75 C12-15 alkyl benzoate 13.7 11.12
11.10 11.00 11.00 11.00 Al--Zr gly in propylene 53.57 58.13 59.57
59.00 59.00 59.00 glycol (28%).sup.a Propylene glycol 0 0 0 2.00
6.00 2.00 SD Alcohol 40 (95%) 0 0 0 0 9.00 9.00 Water 12.13 13.16
11.93 13.00 0 4.00 NaCl 2.0 2.17 2.00 0 0 0 Fragrance 1.0 1.0 1.0
1.0 1.0 1.0 Oleth-20 0.5 0.54 0.5 0 0 0 Dimethicone (Dow Corning 0
0.81 0 0 0 0 200 Fluid (50 centistokes) Initial complex 210-220
125-135 n.d. 170-180 90-100 100-110 viscosity (CarriMed) Pa sec Pa
sec Pa sec Pa sec Pa sec Complex Viscosity (after 2 n.d. n.d. n.d.
90-100 40-45 115-130 weeks at 49.degree. C.) Pa sec Pa sec Pa sec
Complex Viscosity (after 4 280-295 n.d. n.d. 70-80 65-70 170-180
weeks at 49.degree. C.) Pa sec Pa sec Pa sec Pa sec Conductivity
727 819 n.d. n.d. n.d. n.d. .sup.aWestchlor 4105 used for Examples
25 A-C.
Examples 28-34
[0306] The method of Example 1 may be used to make compositions
using the following ingredients as shown in Table VI. The items
listed above the antiperspirant active are used for the external
phase and the ingredients from the antiperspirant ingredient down
are used for the internal phase. Batches can be made in 500 g
quantities.
6TABLE VI Ingredient Ex. 28 Ex. 29 Ex. 30 Ex. 31 Ex. 32 Ex. 33 Ex.
34 C12-15 alkyl 10.40 10.00 9.10 9.25 8.25 9.25 9.30 benzoate.sup.a
Cyclomethicone (D5) 7.10 7.50 10.90 8.75 9.75 8.75 8.20 Neopentyl
glycol 0 2.00 4.00 2.00 4.00 0 diheptanoate PEG-8 laurate.sup.e 0 0
2.00 0 0 0 0 Isocetyl stearate.sup.h 0 0 0 0 2.00 0 0 Dimethicone
copolyol 0 0 0 0 0 0 2.00 laurate.sup.i 40% dimethicone 5.50 5.50
3.00 3.00 3.00 3.00 5.50 copolyol (in cyclomethicone)
Antiperspirant active.sup.b 59.00 59.00 59.00 53.50 59.00 59.00
59.00 Water 13.00 13.00 13.00 4.00 13.00 4.00 13.00
PPG-12-buteth-16.sup.c 4.00 0 0 0 0 0 0 Propylene glycol 0 2.00
2.00 0 2.00 2.00 2.00 Tripropylene glycol 0 0 0 4.50 0 0 0 Ethanol
(95%) 0 0 0 9.00 0 9.00 0 Cosmetic wax.sup.g 0 0 0 3.00 0 0 0
Fragrance.sup.d 1.00 1.00 1.00 1.00 1.00 0 1.00 Initial
viscosity.sup.f .sup.aFINSOLV TN. .sup.bWESTCHLOR A2Z 4105 (28%
propylene glycol and 5.5% glycine). .sup.cUCON 50-660 from Amerchol
Corp. .sup.dAdd as a separate ingredient to either phase or at the
end. .sup.eJEEMATE 400 ML from Jeen International Corp.
.sup.fBrookfield method as described above will give values in the
range of 160,000-230 centipoise. .sup.gDOW CORNING 2501 cosmetic
wax (dimethicone copolyol). .sup.hCrodanol ICS from Croda, Inc.
.sup.iSILWAX WSL from Siltech Corp.
Examples 35-40
[0307] The method of Example 1 may be used to make compositions
using the following ingredients as shown in Table VII. The items
listed above the antiperspirant active are used for the external
phase and the ingredients from the antiperspirant ingredient down
are used for the internal phase. Batches can be made in 500 g
quantities.
7TABLE VII Ingredient Ex. 35 Ex. 36 Ex. 37 Ex. 38 Ex. 39 Ex. 40
C12-15 Alkyl benzoate.sup.a 7.70 9.00 7.30 12.00 10.40 7.90
Cyclomethicone.sup.b 4.30 10.00 7.70 10.00 9.80 15.10 Neopentyl
glycol diheptanoate 8.00 4.00 0 0 0 0 PPG-10-cetyl ether.sup.f 0 0
5.00 3.00 0 0 Dimethicone.sup.g (50 centistokes) 0 0 0 0 0.80 1.00
40% dimethicone copolyol (in 5.00 6.00 5.00 5.00 4.00 5.00
cyclomethicone) Antiperspirant active.sup.c 59.00 35.72 59.00 50.00
59.00 54.00 Water 3.00 0 13.00 12.70 13.00 0 NaCl.sup.h 0 0 0 2.00
0 0 Propylene glycol 0 7.15 2.00 3.80 2.00 16.00 Tripropylene
glycol 2.00 17.51 0 0 0 0 Ethanol (95%) 10.00 9.12 0 0 0 0
Polysorbate 80 0 0.50 0 0 0 0 Oleth-20 0 0 0.50 0 0 Fragrance.sup.d
1.00 1.00 1.00 1.00 1.00 1.00 Initial viscosity.sup.e 220,000
230,000 110,000 200,000 300,000 170,000 .sup.aFINSOLV TN. .sup.bDow
Cornng 245. .sup.cWESTCHLOR A2Z 4105 (28% propylene glycol and 5.5%
glycine) for Examples 35, 37 and 39; WESTCHLOR ZR 40BX3 (42% ACT,
29% propylene glycol and 29% water) for Example 36; WESTCHLOR 35B
(30% propylene glycol and 5.1% glycine) for Example 38; and REZAL
36 GP for Example 40. .sup.dAdd as a separate ingredient to either
phase or at the end. .sup.eBrookfield method as described above.
Unit is centipoise. .sup.fPROCETYL 10 from Croda. .sup.gDOWCORNING
200 Fluid. .sup.hNaCl is premixed with water in Ex. 38 before
addition.
Examples 45-48
[0308] The method of Example 2 may be used to make compositions
using the following ingredients as shown in Table VIII. The items
listed above the antiperspirant active are used for the external
phase and the ingredients from the antiperspirant ingredient down
are used for the internal phase. Batches can be made in 500 g
quantities.
8TABLE VIII Ingredient Ex. 45 Ex. 46 Ex. 47 Ex. 48 C12-15 Alkyl
benzoate.sup.a 7.25 6.90 6.35 0 Cyclomethicone.sup.b 6.75 7.10 7.65
4.00 Triethylhexanoin.sup.f 4.00 0 0 0 Ethyl hexyl
isostearate.sup.h 0 0 0 0 Silicone elastomer in 6.00 6.00 6.00 8.00
cyclomethicone.sup.g Glyceryl oleate in propylene 0 0 4.00 0
glycol.sup.i Neopentyl glycol diheptanoate 0 0 0 4.00 Isopropyl
isostearate 0 0 0 8.00 40% dimethicone copolyol (in 5.00 5.00 5.00
5.00 cyclomethicone) Antiperspirant active.sup.c 35.00 35.00 35.00
32.15 Water 0 0 0 6.62 Propylene glycol 17.00 17.00 17.00 0
Tripropylene glycol 8.25 8.25 8.25 21.00 Ethanol (95%) 9.52 9.52
9.52 10.00 Polysorbate 80 0.23 0.23 0.23 0.23 Fragrance.sup.d 1.00
1.00 1.00 1.00 Initial viscosity.sup.e .sup.a = FINSOLV TN. .sup.b
= Dow Corning 245. .sup.c = WESTCHLOR A2Z 4105 (28% propylene
glycol and 5.5% glycine) for Example 48; and WESTCHLOR ZR 40BX3
(42% ACT, 29% propylene glycol and 29% water) for Examples 45-47
.sup.d = Add as a separate ingredient to either phase or at the
end. .sup.e = Brookfield method as described above and will give
values in the range of 180,000-220,000 centipoise. .sup.f = ESTOL
3609 from Uniquema. .sup.g = Elastomer as described in U.S. Pat.
No. 6,060,546 at a concentration of 5.8% solids in cyclomethicone.
This patent is incorporated by reference for the description of the
elastomer. .sup.h = PRISORINE 2036 from Uniquema. .sup.i = ARLACEL
186 from Uniquema.
* * * * *