Note: Descriptions are shown in the official language in which they were submitted.
~ W 0 94/10968 ~ 1 ~ 4 7 ~ ~ PCT/US93/11174
.
-- 1 --
COMPOSITIONS AND METHODS FOR TEMPORARILY COLORING HAIR USING
SOLUBILIZED MELANIN
This application is a continuation-in-part to U.S.S.N.
07/978,611 filed November 19, 1992.
BAC~GRO~ND OF T~ 1~,V~. ~U..
This invention relates to compositions and methods
for temporarily coloring hair using a melAnin derivative
that is obt~i n~l by chemi~A lly modifying melanin to
impart water solubility, which mel An in derivative is
characterized by anionic substituent groups when
solubilized.
Melanin is the naturally G~11 ing pigment that
gives hair its color. A general ~isctlccion of the
properties and chemistry Of mel:~n;r~c may be found in
Prota, P~G~e38 Tn The Che~ictry Of Melanins And Related
Metabolites, Med. Res. Reviews, 8:525-56 (1988) and
Moncrieff, Manufacturing Chemist, XXI, 8:330-34 (August
1950). The gradual loss of mel~r~in~ with age, causes
hair to turn gray. Altho~gh gray hair can be colored
using chemical dyes, most people prefer to dye their hair
with natural pigments, such as melAni~-hA~^~ dyes.
In the past, one of the be~t natural pigment methods
for permanently coloring gray hair involved the use of
melanin precursors (such as 5,6 dihydroxyindole (DHI))
that when combined with an oY;~t or a metal salt, form
melanin pigments within the hair shaft. See, for
example, U.S. Patent 3,194,734 (Seemuller et al.), U.S.
Patent 4,808,190 (Grollier et al.), and U.S. Patent
4,888,027 (Grollier et al.). However, the use of these
melanin precursors has many ~is~vantages.
The primary disadvantage is that the hair colors
W094/10968 , PCT/US93/11
2~ 5475~
-- 2
initially producQd with mel~nin precursors are
undesirable achromatic colors (cold grays and blacks).
Melanin precursor-dyed hair must undergo a ~~on~
treatment step with an oxidant such as hydrogen peroxide
to achieve natural chromatic colors (warm yellows, reds,
and browns). See, for example, U.S. Patent 3,194,734
(Seemuller et al.). In addition, melanin precur&ors are
expensive and, becau~e they are highly reactive, are
difficult to work with. The use of melanin precursors
also results in undesirable scalp and skin staining.
Furthermore, because melanin precursors penetrate
into the hair shaft, the hair colors produced using
melanin precursors are permanent hair colors. That is,
hair color muct grow out with the hair. Often, consumers
prefer to use a temporary hair color that will wash out
after one or two shampoos. However, temporary hair
colors are unacceptable to consumers unless they resist
fading in sunlight, do not rub off, and do not bleed when
in contact with perspiration, rain, or swimming pool
water.
Melanin pigment itself is unacceptable for use in a
temporary hair dye composition because it merely coats
the hair shaft without appreciable affinity for the hair
shaft. Consequently, the mel A~i n is easily rubbed off
the hair and leaves hair feeling rough.
Therefore, there exists a need in the art for a
cnmrocition ~hat pro~ e~, in a single treatment step,
temporary natural-looking hair color that will not fade
substantially in sunlight, will not rub off, and will not
bleed when in contac~ with water; is inexpensive; will
not stain skin; and is simple to wor~ with. Applicants
have surprisingly found that an aqueous composition,
~ W094/10968 2 1 5 4 7 ~ O PCT/US93/11174
- 3
comprising a water soluble me~ni n (as hereinafter
r described) and at least one water soluble or water
dispersible cationic material provides a hair coloring
composition suitable to impart a temporary color to hair
that achieves these characteristics.
U.S. Patent 5,006,331 (~ in) discloses the use of
melanin that has been solubilized by triethanolamine and
oxidized by ferric chloride. The re~ultant suspension
mixture of melanin, triethanolamine and ferric chloride
is used to obtain compositions for skin protection, for
wound hP~ q and for streng~hPning hair. In an
alternatc method, the melanin is rendered water soluble
by mildly hydrolyzing the mel~n; ~ using Trypsin in an
alkaline medium for several days at room temperature.
Melanin i~ present in the skin protectant compositions of
ki~ in an amount of from about O.OOl to about 0.09~,
along with from about O.OOOl~ to about 0.27% ferric
chloride, both being on a weight basis. The skin
protectant composition ~urther contains up to about 5~ by
weight triethanolamine. While not providing a range of
concentration for the amount of mel Ani n hydrolysate for
the hair protectant compositions according to her
invention, r,~c~i~ states at column 6, line 30 that it is
present therein in an amount of only about 0.0015% by
weight of the total composition. However, this level of
's melA~in hydrolysate is wholly insufficient to
impart a color to hair. Moreover, neither of ~7A Cki n ~ s
methods provide a mel~ material of an anionic
character.
Wolfram, et al, The Me~h~nicm of Hair Bleaching, J.
Soc. Cosmet. Chem., 2l:875-sO0 (1970), discloses
extraction of melanin from hair by acid hydrolysis, and
considers the reaction of m~l Ani ~ pigment with hydrogen
peroxide. Wolfram isolates the peroxide reacted ~PlAnin
by destroying the peroxide with platinum black after a
WO94/10968 PCT/US93/11 ~
2 ~ 5 ~ 4 -
reaction period of sixty minutes.
PCT Application Wo 91/17738 discloses the use of
soluble mel~nin derivatives in a process for producing
lightly colored mel~n;n~ that are aesthetically suitable
for USQ in cosmetic composition
~ W094/10968 2 1 ~ 4 7 ~ O PCT/US93/11174
8n~Y OF ~ TNVRUTTO~
It i8 an object of this invention to provide an
aqueous composition for temporarily coloring hair using
water soluble melanin derivative~.
It is also an objec~ of this invention to provide a
composition that will produce a temporary natural-loo~ing
hair color that resists fading in sunlight, will not rub
off, and will not bleed when in contact with water.
It is further an object of thi~ invention to provide
an inD~p~n~ive composition for temporarily coloring hair
using water soluble melanin derivatives.
It is also an object of this invention to provide a
compo~ition for temporarily coloring hair comprising
soluble melanin derivatives that do not stain skin.
It is also an object of this invention to provide a
composition that is simple to work with for temporarily
coloring hair using water soluble melanin derivatives.
It is also an object of this invention to provide a
one-step process for temporarily coloring hair.
In accordance with this invention, an aqueous
composition is provided for temporarily coloring hair
comprising water soluble melanin derivatives and at least
one water soluble or water dispersible cationic material.
Processes for temporarily coloring hair using that
composition are also provided.
W094/10968 PCT/US93/1 ~
21547~ 6 -
D~Tr~n n~TPT~ON QF TR~ l~v~
The pre~ent invention provides aqueous compositions
comprising water soluble ma- An; n and at least one water
soluble or water ~i-c~rsible cationic material, which
compositions are suitable for use as temporary hair
colors.
The water soluble r-l Ani n derivatives suitable in
the compositions and methods of the present invention are
hereinafter referred to as ~solubilized mel~ni~ which
terminology is believed ~o be consistent with the
nomenclature used in the Wolfram article and used
generally in the melanin chemigtry art. The solubilized
melanins usaful in the compositions of the present
invention are obtained by chemically modifying melanin in
such manner a~ to impart water golubility. An essential
aspect of the present invention is that the solubilized
melanin in combination with a water soluble or water
dispersible cationic material provides a hair dye
composition which promotes affinity of the solubilized
melanin for the hair. Thus, the solubilized melanin
useful in the present invention is believed to form a
complex with the cationic material that has such affinity
for the hair. It is further believed that the
solubilized melanin contain~ one or more anionic
substituent group that not only aid in its solubilization
but also permit complexation with the cationic material.
Such solubilized melanin i~ hereinafter referred to as
anionic solubilized mel A~i n . Mel An; ni C materials that
are dissoluble in water but which do not complex with a
cationic material, for example, the melanin materials
described in U.S. 5,006,331 to GA~;n, are not suitable
in the compositions of the present invention. Typically,
the solubilized melA~in~ used herein have a water
~ W~94/10968 2 1 5 4 7 ~ O PCT/US93/11174
v - 7 -
solubility of at least 0.1%. While not limiting, the
solubilized mel~ni nC generally do not have a water
solubility in ~Yc~c of about lO~. Generally, the water
solubility ranges from about O.l to about 5%. As used
herein the term '~m~l~ni~ refers to the insolu~le
pigment.
Preferably, the solublized mel~;n of the present
invention is made, 8~ taught by the above-mentioned
Wolfram reference, by reacting melanin with hydrogen
peroxide in dilute aqueous alk~ solution, generally
at room temperature. The Wolfram article is incorporated
herein by reference thereto. The reaction proceeds
typically for 30 minutes to several hours, preferably for
30 to 120 minutes, dep~n~in1 on the source the melanin
and the rQn~q~trations of the reactants. The reaction is
terminated well before the peroYi~ begins to bleach the
melanin species present in the reaction mixture.
It i8 believed, based upon the observations of the
hair dyeinq properties of the compositions of the present
invention, that the peroxide reacts with the melanin in
such manner as to provide carboxylate groups to the
structure of the melanin, which groups are anionic in
aqueous media having a pH above 4, preferably
approximately neutral, and most preferably alkaline.
While solubilized ~1Anin as obtained above may be
isolated by acidification of the aqueous reaction medium,
it is not preferred to do so as there is some evidence to
~ugge~t that solublized melAni~ in solid form ages and is
less suitable in the preparation of the compositions of
the present invention. Accordingly, the soluble melanin
i8 preferably used in the form of dilute aqueous solution
having a pH above 4, preferably from about 6 to about lO,
most preferably from about 7 to about 8. Freshly
-
W094/1~68 PCT/US93/11 ~
2i~4~ 8 -
prepared solubilized melanin in solid form may also be
used with good sl~r~e~.
The solubilized melanin that is useful in this
invention may be ob~ e~ from naturally o~ ing,
chemically synthesized, or ~iosynthetic mel~ni~. Thus,
melAnin~ may be isolated from a variety of natural
sources, including human, pri~te~ bovine and other
animals. In particular, squid melanin (sepia melanin) is
commercially available. As well known in the art
biosynthetic melanin can be made by reaction of dopa and
tyrosinase. Similarly, various synthetic rout~s for
making melanin are known, in particular, by the oxidation
of dopa under controlled conditions. The source of the
melanin is not critical. As used herein, the term
"melanin" refars to the insoluble pigment. The
solubilized melAnin that is suitable for use with this
invention may be obtained by any method that imparts an
anionic character to the melanin molecule, i.e.,
solubilized melanin capable of forming a complex with the
water soluble or water dispersible cationic material.
The amount of solubilized me~ required in the
composition of this invention will vary according to
factors such as the carrier used, the initial hair color
of the cQn~mer prior to dyeing, and the desired end hair
color. Bafied on applicant~s theory of the invention, the
amount of solubilized melanin present in the composition
would also depend upon the degree to which it complexes
with the cationic material, i.e., the extent of anionic
charges present on the melanin molecule. In this regard,
the anionic character of the solubilized melanin obtained
in accordance with the Wolfram article can be varied
n~ i nq upon the severity and extent of the reaction
between melanin and hydrogen peroxide. Thus, a more
W094/10968 ~1 5 4 7 S ~ PCT/US93/11174
soluble material will be obt~i n~ with increasingly
SQVere reaction conditions or longer duration of contact
with peroxide. A tinctorially effective amount of
solubi~ A melanin should be used. In general, however,
the amount of solubilized mel~ni n required is at leaQt
about 0.1~, typically from about 0.1% up to its
solubility limit in the composition, but generally less
than about 5.0%, and preferably from about 0.2 to a~out
3.0~, all concentrations being on a weight basis.
A water soluble or water dispersible cationic
material is the second essQntial constituent of the hair
dye composition, along with the solubilized melanin.
While not wishing to be bound by any particular theory,
it i8 belisved that the cationic material complexes with
the solubilized melanin molecule, especially anionic
solubilized melanin, which complex has an affinity for
hair. Accordingly, the complex imparts a temporary color
to the hair that, in view of its affinity for the hair,
does not bleed when in contact with water. The color is
also resistant to fading by sunlight, does not stain skin
when properly applied to hair, and is easy to use. The
hair color is easily removed by shampooing, which appear~
to negate the affinity of the complex for the hair. By
"water soluble~ or "water dispersible" is meant that an
amount of cationic material sufficient to complex with
the soluble melanin is either dissolved or susr~n~ in
the a~ueous hair dye composition. Generally, the
solubility of the cationic material is at least 0.1 g/100
g of compo~ition, preferably from about 0.5 to 10 g/100 g
of composition.
As hereinafter used, "cationic material" means a
water soluble or water dispersible cationic material.
W094/10968 PCT/US93/11 -
2 15 D~ r~
The cationic materials that may be used in the
pre~ent in~ention must, when combined with the
solubilized melanin, be capable of forming a composition
that is suitable for use as a temporary hair color. That
is, the mixture of cationic material and solubilized
melanin must be either water soluble or water dispersible
under the conditions at which they will be used.
Preferably, the cationic material and 501ubilized melAnin
will form a stable homogen~o~lc solution or emulsion.
Such cationic materials include cationic surface
active agents, cationic surfactants, cationic polymers,
and salts thereof. Compounds that assume a cationic
character at a certain pH are also cationic materials in
accordance with thi~ invention. Suitable cationic
materials that may be used are ~et forth, genQrally, in
the CTFA Cosmetic Ingredient ~nAhook (lst Ed., 1988) at
pages 40-42 (quaternary ~onium compounds) and in
McCutcheon~s Emulsifiers and Detergents (North Amer. Ed.
1987) at page 318 (identifying cationic and amphoteric
surface active materials). Suitability may be determined
by one of ordinary skill in the hair dye art by simple
experimentation. Suitable cationic materials are
positively chargedtetra-substituted nitrogenderivatives
having at least one counterion which is an anionic
moiety, e.g., a halide or methosulfate. Using the
nomenclature of the CTFA ~nAhook~ which is widely used
and accepted by chemists in the cosmetics art, illustra-
tive cationic materials are alkyl trimonium halides,
alkylalkonium halides and the dialkyldimonium halides,
wherein the alkyl group~ have about 10 to about 22
carbons and the halide is Cl or Br, for example,
cetrimonium chloride, dicetyldimonium chloride,
myristrimonium chloride, ~tear~l ko~ i um chloride, etc.;
quaternium compounds, for example, quaternium-16,
W094/10968 2 1 ~ 4 7 5 0 PCT/US93/ill74
quaternium-26, quaternium 60 etc.; polymeric quaternium
compounds, for example, polyquaternium 1, polyquaternium-
6, polyquaternium-7, polyquaternium-11, etc.; cationic
resin3 such as guar hydroxypropyltrimonium chloride and
chitosan; and amphoteric surface active agents such as
sodium coco~mphopropionate. The cationic material should
be water soluble or water dispersible within the
conc~ntration ranges contemplated herein, in order to
effect complexation with the solubilized mel A~i n .
Preferred are the alkyltrimonium and
dialkyldimonium chlorides, especially stearatrimonium
chloride and dicetyldimonium chloride; polyquaternium-6
which is a polymer of dimethyldiallyl a lonium chloride
sold under the trade name Merquat 100; polyquaternium-39
which i~ a terpolymer of acrylic acid, dimethyldiallyl
ammonium chloride and acrylamide sold under the trade
name Merquat 3330 and polyquaternium-ll which is a
polymer obt~in~ by reaction of dimethyl sulfate and a
copolymer of vinyl pyrrolidone and
dimethylaminomethacrylate sold under the trade names
Gafquat 734 and 755.
The cationic material is present in an amount
sufficient to form the aforementio~ complex in the
composition in sufficient cQ~c6~tration to effect the
temporary color to hair. PrQferably, sub~tantially all
of the cationic material and the solubilized me~ are
complexed. Thus, the amount of cationic material presQnt
in the composition will dep~nd on the number of cationic
charges borne by the cationic material, as well as the
number of anionic charges to be neutralized on the
solubilized melanin. While some degree of
experimentation may be required to precisely determine
the amount of cationic material, in general, the com-
WO94/10968 PCT/US93/11 ~
2i5 ~
- 12 -
position should contain from about 0.1 to about 20~,
preferably from about 0.1 to about 10~, most prefereably
from 0.2 to 5% cationic material by weight of the total
composition. The weight ratio of solubilized ~l An i~ to
cationic m2t~rial varie~ widely. In general, this weight
ratio will be from about 1:4 to about 10:1, preferably
from about 1:1 to about 5:1.
The composition of this invention are stable for a
period of time, as demonstrated in Example 9. That is,
hair can be temporarily dyed immediately after the
solubilized mel Ani ~ is combined with the cationic
material, or application of the composition can be
delayed.
Although the pH of the composition may not be so low
or high as to damage hair, the composition is useful at
a wide range of pH values. The correct pH for a
particular composition is a function of the type of
cationic material used and the amount: of solubilized
melanin. In general, however, the pH of the composition
will be abou~ 3 to about 10, preferably 4 to 8.
In addition to the solubilized melanin and the
cationic material, it may be desirable to include
cosmetically acceptable carriers in the compositions of
this invention. Acceptable carriers vary from simple
solutions or dispersions with aqueous or alcoholic
solvents, to complex mixtures that contain thicken; ng
agents. The carriers that may be used in accordance with
this invention must be compatible with solubilized
melanin.
It may also be desirable to include in the
compositions of this invention adjuvants or additives
WO94/10968 21~ 4 7 5 0 PCT/US93/11174
that are commonly found in hair color compositions, in
amounts effectivQ to provide their
int~ function. Such adjuvants or additives include
solvents, solubilizing agents, thickening agents,
alkalizing agents, chelating agents, preservatives and
fragrances .
The solvents that may be used include organic
solvents or solvent system~ that are compatible with
solubilizQd m~lanin. A numbsr of ~rganic solvQnts are
known in the art that are useful for such purposes.
These organic solvents include alcohols, particularly
alkyl alcohols of 1-6 carbons, especially ethanol and
propanol; and glycols of up to about lO carbons,
especially diethyleneglycol, monobutyl ether, carbitols,
and benzyl alcohol.
The thickening agents that may be used in the
compositions of this invention include:
polyvinylpyrrolidone, gum arabic, cellulose derivatives
such as methylcellulose or hydroxyethylcellulose, and
inorganic thirkPners such as bentonite. The additional
solubilizing agents that may be used in the compositions
of this invention include ethoxylated fatty alcohols.
The preservatives that may be used in the
compositions of this invention include: methyl- and
propyl paraben, 2-phenoxyethanol, DMDMH, and Kathon CG.
The hair color compositions of this invention may be
prepared by methods known in the art generally by simple
admixture of the various constituents. However, it is
generally preferred, especially when the final product pH
will be acidic, to use an aqueous solution of the
solubilized melanin. It is further preferred to form a
W094/10968 PCT/US93/11 ~
2i~
- 14 -
premix of the solubilized mel~ni~ and the cationic
material to which the rema; n; nq constituents are added.
This invention also provides a process for
temporarily coloring hair, which comprises applying to
the hair an aqueous composition comprising solubilized
melanin and at least one cationic material. The
compositions may be applied to the hair by conventional
t~r~n;ques known in the art. For example, they can be
poured over the hair or applied with an applicator. ~he
amount of time for which the dye composition must be in
contact with the hair is not critical. It may vary from
about 2 minutes to about 50 minutes, but is usually from
about 5 minutes to abou~ 30 minutes.
In another embodiment of the invention, the hair
may be dyed by forming the hair dye complex obt~;n~ from
the interaction of ~he solubilized melanin and the
cationic material directly on the hair. Thus, the
proces~ may be practiced by applying to the hair two
aqueous compositions sequentially and without
intermediate rinsing, one of said two aqueous
compositions containing the solubilized melanin and the
other containing the cationic material. The hair dyeing
complex is formed on the hair in situ and is evenly
distributed by gentle masgage of the scalp. In this
emhoAiment the amounts of the solubilized melanin and
cationic material are the same as when a single aqueous
composition i8 employed. Accordingly, the concentration5
of both essential constituents are seen to be based on
the total weight of the two separately applied
compositions. Prefe~ably, the composition containing the
cationic material is first applied to the hair, followed
by application of the solubilized melanin-contA;~;ng
composition.
W094/10968 2 1 ~ 4 7 5 0 PCT/US93/11174
The following examples are illustrative of the
present invention and should not be construed as limiting
the scope of this invention in any manner. In each of
the following examples, sepia mel~in was isolated from
cuttlefish ink sac~ and wa~ used to prepare solubilized
mela~in according to the method described in Wolfram, et
al., J. Soc. Cosmetic Chemist, 21:875-900 (1970).
The Hunter tristimulus values used below are
measures of reflected light and describe color using
three parameters: L, a, and b. When L 5 0~ the color is
black, and when L 5 100 ~ the color is white. The more
positive "a" is, the redder the color; the more negative
"a" is, the greener the color. The more positive "b" is,
the yellower the color; the more negative "b" is, the
bluer the color. The Hunter colorimetry device and
system is used widely in evaluating the color of hair.
~Mpr~ ~
40 mg of freshly prepared solubilized mel Ani n in
particulate form wa~ dissolved in 5 ml of water (Solution
l). 40 mg dicetyldimonium chloride was A~ to 5 ml of
water and stirred until homogen-~ ~ (Solution 2).
Solution l wa~ stirred into Solution 2 (Solution 3).
The pH of the lO ml of combined solutions was 7.l.
A tress of Piedmont hair was treated for 2 minute~
with Solution 3. The tress was then blotted dry with
paper and dried with a hair dryer. The tress was
several ch~e~ darker than its original color. The
results are set forth in Table l.
WO94/10968 PCT/US93/11 -
21547~ - 16 -
T~bl~ 1
No. Tr~at~nt co~ttions ~unter Color Values Vt 8ual Color
~ ~ b.
1.1 Undyed Piedmont tress64.3 -0.8 19.3 light blonde
1.2 Dyed Piedmont tress45.4 2.6 14.5 dark blonde
The dyed tress ret~;n~ its color after it was rinsed wi~h
water, but wag restored to its original color after it was
shampooed.
~MPr.R 2
The proce~t~re described in Example 1 was repeated, except,
prior to being applied to the hair, the pH of Solution 3 was
adjusted to 4.4 using 0.1 M ~C1. The results are set forth in
Table 2.
T~hl- 2
No. Treatmont Con~it~on~ ~nter Color Values Vi~ual Col~r
~2
2.1 Undyed Piedmont tress64.3 -0.8 19.3 light blonde
2.2 Dyed Piedmont tress37.5 3.1 11.5 light brown
~aMP~-~ 3
The procedure described in Example 1 was repeated except,
prior to being applied to the hair, the pH of Solution 3 was
adjusted to 9.0 using dilute ammonia. The results are set forth in
~ W094/10968 2 1 5 ~ 7 S O PCT/US93/11174
- 17 -
Table 3.
T~hl- 3
No. Tr~at~^nt Con~ttion~ ~nnt~r Color V~lu~8 Vi8~ Col~
~ a b
3.1 Undyed Piedmont tress 64.3 -0.8 19.3 light blond~
3.2 Dyed Piedmont tress 45.8 2.8 14.7 dark blonde
40 mg of freshly prepared solubilized melanin in particulate
form was dissolved in 5 ml of water (Solution 10). 60 mg of
Polyquaterniu~-11 (Gafquat 755 N) was in 5 ml of water (Solution
20). Solution lo was stirred into solution 20 (solution 30). The
pH of the 10 ml of combined solutions was 7Ø
A tress of Piedmont hair was treated for 2 minutes with
Solution 30. The tress wa~ then blotted dry with paper and dried
with a hair dryer. The rQsults are sQt forth in Table 4.
T~ o 4
Treat~^nt Con~ition~ ~unter Color Values Visual Color
~ a b
4.1 Undyed Piedmont tress 64.3 -0.8 19.3 light blonde
4.2 Dyed Piedmont tress 52.0 1.1 15.1 medium blonde
WO94/10968 PCT/US93/11 ~
2 lS 4r~' S ~ -- 18
~AMPT.~ 5
The ~o~e~ule described in Example 4 was~repeated, except,
prior to being applied to the hair, the pH of Solution 30 was
adjusted to 4.4 u~ing 0.1 M HCl. The results are set forth in
Table 5.
Table 5
NQ. Treatmont Con~ition~ ~unter Color Values Visual Color
~ a b
5.1 Undyed Piedmont tress 64.3 -0.8 19.3 light blonde
5.2 Dyed Piedmont tress 52.7 0.9 15.8 medium ~londe
~Mpr~ 6
20 mg of freshly prepared solubilized melanin in powder form
was dissolved in 3 ml of water (Solution 100). 160 mg of
Polyquaternium-ll (Gafquat 755 N) was dissolved in 3 ml of water
(Solution 200). Solution 100 was stirred into solution 200
(Solution 300). The pH of the 6 ml of combined solutions was 6.8.
A tress of Piedmont hair was treated for 2 minutes with
Solution 300. The tress was then blotted dry with paper and dried
with a hair dryer. The regults are set forth in Table 6.
~ W094/10g68 21~ ~ 7 ~ ~ PCT/US93/11174
- 19 -
~I~hl O 6
No. Tre4t~ent Con~tion~ Eunter Color Valuos Visual Color
; ~ ~ b
6.1 Undyed Piedmont tress 64.3 -0.8 19.3 light blonds
6.2 Dyed Piedmont tres~ 51.9 1.0 14.9 medium blonde
~a~r-~ 7
The procedure described in Example 6 was repeated except,
prior to being applied to the hair, the pH of Solution 300 was
adjusted to 4.5 using 0.1 M HCl. The results are set forth in
Table 7.
~ 7
No. --~nt Con~t~on~~nt ~ Colo~ V~luc8 V'~8~ t COl~--
b
7.1 Undyed Piedmont tre~s 64.3 -0.8 19.3 light blonde
7.2 Dyed Piedmont tres~49.8 1.9 15.3 medium blondl7
~MP~ 8
40 mg of freshly prepared solubilized mel~ni n in particulate
form was dissolved in 5 ml of water (Solution 1). 40 mg of
cationic material was added to 5 ml of water and stirred until
homogeneous (Solution 2). Solution:l was stirred into Solution 2
tSolution 3). The pH of the 10 ml of combined solution was about
7.2 to 7.3.
W094/10968 PCT/US93/11 ~
2 15 ~ 20 -
A tress of Piedmont hair and a tress of gray hair were
treated for 10 minutes with a Solution 3. Each tress was then
blotted dry with paper and dri~d ~ith a hair dryer. The results
are set forth in Table 8.
~'-t~ Piod~t~nt ~a~r Gr~Y ~a~r
~. ~at~riAl ~l-nt~r Color V~lue~ ~nnter color valuo~
~ ~ b ~ ~ k
8.1 Dicetyldimonium 52.6 2.1 16.9 29.9 1.4 6.8
chloride
8.2 Merquat 3330 54.7 1.2 17.0 32.3 0.5 7.3
8.3 Polyquat 11 54.4 1.4 17.5 29.3 0.8 6.1
F~X AMPT.F! 9
Formulation No. 9.1 wa~ prepared by dissolving 40 mg of
Polyquat 11 in 5 ml of watQr (Solution 1). 40 mg of freshly
prepared solubilized melanin in particulate form was dissolved in
5 ml water (Solution 2~. Solutions 1 and 2 were combined (Solution
3).
Formulation No. 9.2 wa~ prepared by dissolving 80 mg of
Polyquat 11 in 5 ml of water (Solution 1). 80 mg of freshly
prepared solubilized melAn;n in particulate form was dissolved in
S ml of water (Solution 2). Solutions 1 and 2 were combined
(Solution 3). Each Formulation was applied to a tress of Piedmont
W094/10968 2 1 ~ ~ 7 5 0 PCT/US93/11174
- 21 -
hair and a tre~s of gray hair for lO minutes, both immediately
and 24 hours after the Formulation wa~ prepared. The appearance of
the solution~ did not change during this time. The diffeL. _e in
hair color b~tween the imm~diate and the 24 hour application is
insignificant. The regults are set forth in Table 9.
T~ Q 9
Applic~tio~ Ti -
Aft~r ~or~ulation El~gmont ~t r ~y ~ t
No. ~ p-o~r~ nt~r Color V~luos Rnnt~r Color Va1u-~
g.l Immediate 52.01.7 16.3 31.5 0.7 6.6
24 hours 54.01.3 17.7 31.4 l.0 6.8
9.2 Immediate 50.82.0 l5.9 28.4 1.4 6.5
24 hours 48.72.1 l5.0 29.5 1.3 6.7
Control Tress 68.3-0.8 21.2 33.9 0.3 7.6
It will be apparent to those skilled in the art that the
invention described herein can be practiced by other than the
~mbodimQnts disclosQd herQin, which are presented for the pUl~ -e~
of illustration and not of limitation, and the present invention is
limited only by the claims that follow.
