Generally, t
he present disclosure relates to
shampoo compositions
. Particularly, it relates to
waterless (dry)
shampoo composition
s
.
More particula
rly, it relates to alcohol
-
free
and
5
paraben
-
free
waterless (dry)
shampoo composition
s
.
BACKGROUND OF THE
INVENTION
Shampooing forms an essential part of hair care in today’s society.
Shampoos can broadly be
classified i
nto two types: wet shampoos and waterless (dry)
shampoos.
While wet shampoos are quite efficient, they require the use of water, which is an e
xtremely
10
precious resource. Further, wet shampoo compositions generally contain alcohol
and
parabens
, which
may
cause hair
dry
ness
and adverse health effects (depending on the
concentration), respectively
.
Moreover, w
et shampoos are often
required to be
used in
conjunction with conditioners, which give the hair a shiny look and help in maintaining the
pH balance of the hair.
15
Waterless
shampoos
(also known as
dry
shampoos)
, on the other hand,
are a great way to
reduce the use
of water
in hair maintenance.
Since no water is required,
waterless (dry)
shampoos can be used even by people living in areas where water is scarce,
including
campers, backpackers, defence personnel in remote areas, and the like.
However, existing
dry
shampoos are largely inefficient in removing odour, dirt,
sweat
, and
20
oil. Further, unlike wet shampoos, they leave behind residue that is difficult to remove. Due
to these reasons,
dry
shampoos have not become popular with consumers.
There is the
refore, a
need in the art for
a
waterless (dry)
shampoo
composition
that does not
contain alcohol
and paraben
.
There is the
refore, a need in the art for
a
waterless (dry)
shampoo composition that cleans the
25
hair completely without leaving behind any
undesirable
residue.
There is the
refore, a need in the art for
a
waterless (dry)
shampoo composition that can also
condition the hair, thereby
giving
the hair a shiny look
, in addition to maintaining the pH of
the hair
.
SUMMARY OF THE INVENTION
30
In order to overcome
th
e above mentioned drawbacks, alcoh
ol
-
free
and paraben
-
free
waterless (dry)
shampoo compositions are
disclosed, said alcohol
-
free
and paraben
-
free
waterless (dry)
shampoo composition
s
consisting of
87% to 96
%
of
water as a solvent
,
1.5%
to 3.5
%
of a
primary
surfactant,
0.5
%
to 2
%
of a secondary surfactant, 0.05
%
to 2
%
of a first
preservative,
0.05% to 2
%
of a second preservative,
0.025% to 0.1% of a third preservative,
35
3
1
%
to 2.8
%
of a moisturizer, 0.5% to 2% of a viscosity controlling agent,
0.0025% to 0.01
%
of a skin conditioning agent, 0.025% to 0.1% of a chelating agent
and
0.1
% of a fragrance
.
The
primary
surfactant is selected from the group consisting of t
riethanolamine lauryl sulfate
,
a
lkyl benzene sulfonates, lauric acid
salts
, stearic acid
, alkyl
ether sulfates, c
oconut
amine
oxide, dodecyl dimethyl amine oxide
and
N
-
alkyl aminoacids
.
5
The secondary surfactant is selected from the group consisting of c
ocamidopropyl betaine
,
coco betaine, lauryl hydroxypropyl sultaine, coco hydroxypropyl sultaine, di
sodium
cocoamphodiacetate, cocamide MEA and decyl glucoside
.
The first preservative
, the second preservative and the third preservative
are
selected from the
group consisting of
dehydroacetic acid, benzoic acid, sorbic acid, DMDM Hydanto
in and
10
phenoxyethan
ol
isothiazolinone
.
The moisturizer is selected from the group consisting of propylene glycol, glycerine, plant
oils and panthenol.
The
viscosity controlling agent is selected from the group consisting of benzyl alcohol,
sodium polyaconate and tetrasodium
glutamate diacetate.
15
The skin conditioning agent is selected from the group consisting of tocopherol and Vitamin
E.
The chelating agent is selected from the group consisting of
disodium EDTA, polyaspartic
acid and ethylene diamine
-
disuccinic acid.
DETAILED
DESCRIPTION OF THE INVENTION
20
Unless otherwise specified, all the percentages disclosed are
in
w/v.
A
lcohol
-
free
and paraben
-
free
waterless (dry)
shampoo composition
s
are disclosed, said
composition
s consisting
of
87% to 96% of water as a solvent, 1.5% to
3.5% of a primary
surfactant, 0.5% to 2% of a secondary surfactant, 0.05% to 2% of a first preservative, 0.05%
to 2% of a second preservative, 0.025% to 0.1% of a third preservative, 1% to 2.8% of a
25
moisturizer, 0.5% to 2% of a viscosity controlling agen
t, 0.0025% to 0.01% of a skin
conditioning agent, 0.025% to 0.1% of a chelating agent and 0.1% of a fragrance.
In a preferred
embodiment of the present disclosure, the solvent is water.
In
an
embodiment of the present disclosure, the
primary
surfactant is
selected from the group
consisting
of t
riethanolamine lauryl sulfate
, a
lkyl benzene sulfonates, lauric acid
salts
, stearic
30
acid
, alkyl ether sulfates, c
oconut
amine oxide, dodecyl dimethyl amine oxide and
N
-
alkyl
aminoacids
.
In another
preferred
embodiment
of the present disclosure, the
primary
surfactant is
t
riethanolamine lauryl sulfate
.
4
In another embodiment of the present disclosure, the secondary surfactant is selected from the
group consisting of
c
ocamidopropyl betaine
, coco betaine, lauryl hydroxypro
pyl sultaine,
coco hydroxypropyl sultaine, disodium cocoamphodiacetate, cocamide MEA and decyl
glucoside.
In yet another
preferred
embodiment of the present disclosure, the secondary surfactant is
5
c
ocamidopropyl betaine
.
In yet another embodiment of the pr
esent disclosure
, the first preservative is selected from the
group consisting of
dehydroacetic acid, benzoic acid, sorbic acid, DMDM Hydantoin and
phenoxyethanol
isothiazolinone
.
In yet another
preferred
embodiment of the present disclosure, the first preservative is
10
dehydroacetic acid
.
In yet another embodiment of the present disclosure, the second preservative is selected from
the group consisting of
dehydroacetic acid, benzoic acid, sorbic acid, DMDM Hy
dantoin and
phenoxyethanol
isothiazolinone
.
In yet another
preferred
embodiment of the present disclosure, the second preservative is
15
benzoic acid
.
In yet another embodiment of the present disclosure, the third preservative is selected from
the group consi
sting of
dehydroacetic acid, benzoic acid, sorbic acid, DMDM Hydantoin and
phenoxyethanol
isothiazolinone
.
In yet another
preferred
embodiment of the present disclosure, the third preservative is
sorbic
20
acid
.
In yet another embodiment of the present disclo
sure, the moisturizer is selected from the
group consisting of propylene glycol, glycerine, plant oils and panthenol.
In yet another
preferred
embodiment of the present disclosure, the moisturizer is propylene
glycol.
25
In yet another embodiment
of the prese
nt disclosure, the viscosity controlling agent is
selected from the group consisting of benzyl alcohol, sodium polyaconate and tetrasodium
glutamate diacetate.
In yet another
preferred
embodiment of the present disclosure, the
viscosity controlling agent
i
s benzyl alcohol
.
30
In yet another embodiment of the present disclosure, the skin conditioning agent is selected
from the group consisting of tocopherol and Vitamin E.
In yet another preferred embodiment of the present disclosure, the skin conditioning agent
is
tocopherol.
5
In yet another embodiment of the present disclosure, the chelating agent is selected from the
group consisting of disodium EDTA, polyaspartic acid and ethylene diamine
-
disuccinic acid.
In yet another preferred embodiment of the present disc
losure, the chelating agent is
disodium EDTA.
The composition
also
contain
s
a
fragrance. The incorporation of fragrances in shampoos is
5
well established and those skill
ed
in the art would be able to select a suitable fragrance to
achieve the desired
scent.
In yet another embodiment of the present disclosure, the fragrance is a
natural fragrance
(
fragrant compounds that are derived from natural sources
)
.
In yet another embodiment of the present disclosure, the fragrance is a
synthetically produced
10
fragrance
.
In a more preferred embodiment of the present disclosure, the disclosed alcohol
-
free
and
paraben
-
free
waterless (dry)
sh
ampoo compositions consist of 87% to 96% of water, 1.5% to
3.5% of t
riethanolamine lauryl sulfate
, 0.5% to 2% of c
ocamidopropyl betai
ne
, 0.05% to 2%
of dehydroacetic acid, 0.05% to 2% of benzoic acid, 0.025% to 0.1% of sorbic acid, 1% to
15
2.8% of propylene glycol, 0.5% to 2% of benzyl alcohol, 0.0025% to 0.01% of tocopherol,
0.025% to 0.1% of disodium EDTA and 0.1% of the fragrance.
In a most preferred embodiment of the present disclosure, the disclosed alcohol
-
free
and
paraben
-
free
waterless (dry)
shampoo compositions consist of
93.59% of water, 2.5% of
t
riethanolamine lauryl sulfate
, 1% of c
ocamidopropyl betaine
, 0.1% of dehydroacet
ic acid,
20
0.1% of benzoic acid, 0.05% of sorbic acid, 1.5% of propylene glycol, 1% of benzyl alcohol,
0.005% of tocopherol, 0.05% of disodium EDTA and 0.1% of the fragrance.
The
disclosed alcohol
-
free
and paraben
-
free
waterless
(dry)
shampoo compositions
are to be
used as given below
:
1.
Apply
onto hair until the hair is completely wet;
25
2.
Gently massage
o
nto the hair;
3.
Dry the hair thoroughly by wiping it with a soft towel;
4.
Repeat the above steps for heavily soiled hair.
The alcohol
-
free
and paraben
-
free
waterle
ss (dry)
shampoo compositions disclosed herein
leave behind no residue, maintain the smoothness of the hair, maintain the
pH of the scalp, do
30
not cause hair dry
ness, completely clean the hair b
y
removing dirt,
sweat
, oil and odour,
provide excellent hair c
onditioning and reduce the microbiological count.
The process by which
the compositions are manufactured consists of mixing the
primary
surfactant and the secondary surfactant
first in a vessel
.
The solvent, the first preservative, the
second
preservative
and the third preservative
are mixed in
a
separate vessel.
The two
35
mixtures are subsequently mixed together and cooled down. Finally, the fragrance is added.
6
For the
examples
disclosed below
, the
viscosity was tested
using the below described
procedure
:
A
quantity of oil (
20
0
C
+
0.1
0
) was placed in a filling tube and transferred to a capillary tube
by gentle suction, taking care to prevent bubble formation in the liquid by keeping the air
vent tube closed. The meniscus of the column of liquid in the capilla
ry tube was adjusted to
5
the level of the top graduation line. Both the vent and the capillary tubes were opened in
order to permit the liquid to flow into the reservoir against atmospheric pressure. The time, in
seconds, for the liquid to flow from the upp
er mark to the lower mark in the capillary tube
was recorded.
The viscometer constant, k, was calculated from the equation:
10
k = v/dt
where,
v is the known viscosity of the liquid in centipoise,
d is the specific gravity of the liquid tested at
20
0
C
, and
t
is the time in seconds for the liquid to pass from the upper mark to the lower mark.
15
Example 1
:
A composition consisting of
90.4% of water, 6.2% of
t
riethanolamine lauryl sulfate, 1
% of
cocamidopropyl betaine
, 0.4% of citric acid and 2% of propylene glycol
did not produce the
required amount of foam for it to be user
-
friendly.
Example 2:
20
A composition consisting of 90.4% of water, 5% of
t
riethanolamine lauryl sulfate, 1
% of
cocamidopropyl betaine
, 1.2% of disodium EDTA, 0.4% of citric acid and 2% of propyle
ne
glycol produced a good amount of foam. However, the composition was found to possess a
high viscosity.
Example 3:
25
A composition consisting of 91.4% of water, 4% of
t
riethanolamine lauryl sulfate, 1
% of
cocamidopropyl betaine
, 0.2% of disodium EDTA, 1% o
f benzyl alcohol, 0.4% of citric acid
and 2% of propylene glycol produced a good amount of foam. However, the foam could not
be removed without the use of water.
Example 4:
30
A composition consisting of 9
3.595
% of water,
2.5
% of
t
riethanolamine lauryl
sulfate, 1
% of
cocamidopropyl betaine
, 0
.05
% of disodium EDTA, 1% of benzyl alcohol,
0.005
% of
tocopherol
,
1.5% of propylene glycol
, 0.1% of dehydroacetic acid, 0.1% of benzoic acid,
7
0.05% of sorbic acid and 0.1% of a fragrance
was found to yield a fresh a
nd clear liquid
having a good viscosity
.
The results of
stability
tests conducted on the composition
disclosed in Example 4
over
one
month
are summarized below:
Attribute
Acceptable Result
Initial Result
Result after
a month
Appearance
Clean, Fresh,
Clear
Liquid
Clean, Fresh, Clear
Liquid
Clean, Fresh,
Clear Liquid
Viscosity
About 1.2
2
centipoise (cps) at
room temperature
1.20
cps
1.21
cps
pH
at 25ºC
5.5 to 6.5
6.2
6.2
Microbial limits

Total Aerobic
microbial Count

Total Mould and
yeast count

E.coli

Salmonella

Pseudomonas
NMT 100 cfu/ml
NMT 10 cfu/ml
Absent
Absent
Absent
< 21cfu/ml
< 1cfu/ml
Absent
Absent
Absent
NA
5
The pH was determined potentiometrically
b
y
means of
a
glass elec
trode and a suitable pH
meter (d
igital).
After setting t
he
pH
meter at
25ºC
,
the pH meter
was standardized
using
standard buffer solutions of pH
value 6.0 and 7.0.
The
pH
of the shampoo was then
measured.
The microbial limits were determined
using the below mentioned protocol
.
10
Pre
-
treatment of the sample:
10 g of the preparation under examination
was suspended
in buffered sodium chloride
-
peptone solution
(
pH 7.0
)
or any other suitable medium shown to ha
ve no antimicrobial
activity.
T
he volume
was adjusted to
100 ml with the same.
A s
uitable surface active
agent
such as 0.1% w/v solution of Polysorbate 80
was added (where required)
to assist
with
the
15
suspension of poorly wettable substances.
8
Inactivation of antimicrobial activity:
For
test specimen
s
known to contain
antimicrobial
substances
,
a corresponding
inactivating agent
was used
to neutralize the antimicrobial
activity. The inactivating agent (Polysorbate 80)
was added to the
chosen diluent preferably
before sterilization.
A
ll th
e necessary items required
for the testing were
kept under a laminar air f
low (LAF)
.
5
T
he pre
-
sterilized petri dish
was labelled
with glass marker,
to
show the media name
(
soyabean casein digest
agar (SCDA) for bacterial count or
Sabouraud Dextrose agar (SDA)
for fungal count
)
,
the name of the product
,
the batch number
and
the
da
te of analysis.
E
ach of 1 ml of pre
-
treated sample
was carefully pipetted
on
to
previously labelled
p
etri dish
in duplicate, said petri dish being maintained under a laminar air flow
.
10
Positive control:
K
nown volume of cells (10
-
10 cells) of
E.coli/ S.aureus
was added in
SCDA plate and allowed to solidify for 30 minutes s. Likewise, known volume of cells of
Candida albicans
was added
in SDA plate
allowed to solidify for 30 minutes
.
Negative Control:
SCDA/ SDA media
was poured
in pre
-
sterilized and labeled pla
tes and
allow to solidify.
15
T
he plates
were incubated
at respective temperature
s
(SCDA
–
35
0
C
-
37
0
C/ SDA 20
0
C
–
25
0
C) for 1
20 hours
(5 days).
The incubate
d
plates
were
monitored every 2
4 hours
.
Calculation
:
Average No. of colonies X Dilution factor
20
CFU / g =
-----------------------------------------------------------
Weight
of sample
It was ensured that the n
egative control
did
not show any growth
at the end of the incubation
period.
Pathogens test:
The pathogens mainly comprise
of
E.coli
,
Salmonella
,
S.aureus
and
25
P.aeruginosa
.
Sample preparation
: 10 gm sample
was aseptically transferred
into sterile 90 ml SCDM
broth.
T
he media
was labelled
with
th
e
media name,
the product batch number
and
the
incubation
date and incubate
d
at 30
0
C
–
35
0
C for 18
-
24 hours
. After
the
incubation
,
if the media was
30
clear
,
it was
conclud
ed that
pathogens are absent. If
turbidity was
observed
,
then
specific
testing of
pathogens
was carried out
as described below:
E.coli
:
9
Primary test:
0.1ml of enrichment media
was transferred
into 10ml of MacConkey’s broth
containing inverted Durham’s tube and incubate
d
at 30
0
C
–
37
0
C for 24 hours to 48 hours
.
T
he tube
was labelled to
show enrichment transfers (SCDM to MacConkey broth), sample
n
umber
and
the
date of enrichment and
incubate
d
at 30
0
C
–
37
0
C for 24 hours
.
After i
ncubation, if Durhams tube showed
gas and
if a
colour change to yellow
occurred
, then
5
a loopful of the same
was
streaked
on MacConkey agar plate and incubate
d for 24
–
72 hours
at 30
0
C
–
37
0
C. If no change
was observed, then the testing was stopped
.
Upon incubation,
the plate was observed
for
typical culture characteristics of
E.coli
. If typical
characteristics wer
e found, then secondary test was conducted.
If
no typical characteristics were found,
the result was recorded
as
‘
Absent
’
for
E.coli.
10
Secondary test (Indole test):
0.5 ml kovac’s reagent
was added
in to pre
-
incubated 5 ml
peptone water (1%).
After
shaking, it was a
llow
ed to stand for 1 minute
,
the formation of a pink colo
u
red ring was
interpreted as a positive result
.
15
The presence of acid and gas and of indole in the secondary test indicates the presence of
E.coli.
Cultural characteristics of
E.coli
in MacConkey agar is as follows:
MacConkey agar plate
Brick red, colonies may have surrounding
zone of precipitated bile.
Salmonella
:
20
0.1 ml of primary enrichment from SCDM
was aseptically transferred
into 10 ml of sterilized
Selenite
-
F
-
Broth or 10 ml
of Tetrathionate Brilliant green Broth tube.
T
he tube
was labelled to
show the enrichment transfers (SCDM to SFB/ SCDM to
TTBGB),
product identification and d
ate of Enrichment
and
incubate
d
at 35
0
C
–
37
0
C for 24 h
ou
rs.
After the incubation period,
if the S
FB tube showed
tur
bidity and the TTBGB tubes showed
25
disappearance of green colour with white precipitate
,
the
n loopful
of
enrichment
was picked
up
and streak
ed
on surface of pre
-
incubated Bismuth sulfite agar (BSA)/ Brilliant Green Agar
(BGA) Media plates/ Xylose lysine Deoxycholate agar/ Deoxycholate agar plate.
T
he plate
was labelled to
show
e
nrichment transfers, (SFB to
BGA/ SFB to BSA/ TTBGB to BSA)
product
identification and d
ate of streak
ing
.
30
10
Upon i
ncubation,
if the plate showed
typical cultural characteristics of
Salmonella
,
b
iochemical identification test
was conducted to confirm the same
.
Secondary test (TSI test):
A
ny colonies showing the
typical
charac
teristics
were sub
-
cultured
in triple sugar iron agar
by first inoculating the surface of the slope with inoculating needle and then making a stab
5
cultures with the same inoculating needle.
T
hese two tubes
were incubated
at 35
0
C
–
37
0
C for 18
-
24 h
ou
rs.
A
fter incubation, yellow butt (acidic) with pink slant (alkaline)
,
with or without
concomitant
blackening of butt from H
2
S p
roduction in TSI tubes indicated
the presence of
Salmonella
.
The
cultural
characteristics of
Salmonella
in media plates are
as follows:
10
Sr. No.
Medium
Description of colony
1
Bismuth Sulphite agar
Black or green
2
Brilliant green agar
Small
, transparent and colourless or opaque,
pinkish or white (frequently surrounded by a
pink or red zone)
3
Deoxycholate citrate agar
Colourless and opaque with or without black
centres.
4
Xylose
-
lysine Deoxycholate agar
Red with or without black centres.
Test for
Staphylococcus aureus
(
S. aureus
):
Upon incubation
,
the growth
was observed
in tube.
Loopful of
e
nrichment
was picked up
and
streak
ed
on the surface of pre
-
incubated Mannitol Salt agar (MSA) media plate. Finally, the
15
plate
s were incubated
at 35
0
C
–
37
0
C for 24
–
48 h
ou
rs.
After the incubation period, the colony morphology
was observed for
typical cultural
characteristics of
S.aureus
.
If typical characteristics were observed, then the presence of
S.aureus
was confirmed by biochemical identification test.
Secondary test:
T
he typical colony of
S.aureus
was streaked
from Mannitol salt agar to
20
Baired Parker agar
and i
ncubate
d
at 35
0
C
–
37
0
C for 24
-
48 h
ou
rs.
After Incubation
,
the growth was examined for black colouration.
If growth showed black
colouration, it was interpreted to as a positive result
.
C
ultural characteristics of
S.aureus
in
MSA/ Baired parker agar plates are
as follows:
MSA plate
Yellow colonies with yellow surrounding
11
zone
Baired Parker agar plate
Black colonies surrounded by clear zone
Test for
Pseudomonas aeruginosa
(
P.aeruginosa
):
L
oopful of enriched SCDM broth
was picked up
and streak
ed
on the surfac
e of pre
-
incubated Cetrimide Agar (CA) media plate.
The plate was labelled to
show the enrichment transfer, (SCDM to CA) product identification
5
and date of streak
ing
. Finally
,
the plate was incubated
at 35
0
C
–
37
0
C for 24
-
72 h
ou
rs.
Upon examination,
if
none of the colonies conformed
to the description given in following
table,
it confirmed the absence
of
Pseudomonas
.
Medium
Description of colony
Cetrimide
Greenish
If any colonies conform
ed
to the description given in above table,
oxidase test was carried out
10
to confirm the presence of
Pseudomonas
.
Oxidase test:
An
isolated colony
was spread well
on oxidase disc from
Cetrimide
agar plate.
The production of
p
urple colour within 5 to 10 seconds
indicated a positive result.
It will be apparent to a person skilled in the art that the above description is for illustrative
15
purposes only and should not be considered as limiting. Various modifications, additions,
alterations and improvements without deviating from the spirit and t
he scope of the
disclosure
may be made by a person skilled in the art.
Such modifications, additions,
alterations
and improvements should be construed as being within the scope of this
disclosure.

Claims:1. An alcohol-free and paraben-free waterless shampoo composition, consisting of:
water as a solvent;
a primary surfactant selected from the group consisting of triethanolamine lauryl sulfate, alkyl benzene sulfonates, lauric acid salts, stearic acid, alkyl ether sulfates, coconut amine oxide, dodecyl dimethyl amine oxide and N-alkyl aminoacids;
a secondary surfactant selected from the group consisting of cocamidopropyl betaine, coco betaine, lauryl hydroxypropyl sultaine, coco hydroxypropyl sultaine, disodium cocoamphodiacetate, cocamide MEA and decyl glucoside;
a first preservative, a second preservative and a third preservative, said first preservative, said second preservative and said third preservative being selected from the group consisting of dehydroacetic acid, benzoic acid, sorbic acid, DMDM Hydantoin and phenoxyethanol isothiazolinone;
a moisturizer selected from the group consisting of propylene glycol, glycerine, plant oils and panthenol;
a viscosity controlling agent selected from the group consisting of benzyl alcohol, sodium polyaconate and tetrasodium glutamate diacetate;
a skin conditioning agent selected from the group consisting of tocopherol and Vitamin E;
a chelating agent selected from the group consisting of disodium EDTA, polyaspartic acid and ethylene diamine-disuccinic acid; and
a fragrance,
wherein the composition consists of:
of 87% to 96% of water, 1.5% to 3.5% of the primary surfactant, 0.5% to 2% of the secondary surfactant, 0.05% to 2% of the first preservative, 0.05% to 2% of the second preservative, 0.025% to 0.1% of the third preservative, 1% to 2.8% of the moisturizer, 0.5% to 2% of the viscosity controlling agent, 0.0025% to 0.01% of the skin conditioning agent, 0.025% to 0.1% of the chelating agent and 0.1% of the fragrance.

2. An alcohol-free and paraben-free waterless shampoo composition according to claim 1, wherein the primary surfactant is triethanolamine lauryl sulfate.

3. An alcohol-free and paraben-free waterless shampoo composition according to claim 1, wherein the secondary surfactant is cocamidopropyl betaine.

4. An alcohol-free and paraben-free waterless shampoo composition according to claim 1, wherein the first preservative is dehydroacetic acid.

5. An alcohol-free and paraben-free waterless shampoo composition according to claim 1, wherein the second preservative is benzoic acid.

6. An alcohol-free and paraben-free waterless shampoo composition according to claim 1, wherein the third preservative is sorbic acid.

7. An alcohol-free and paraben-free waterless shampoo composition according to claim 1, wherein the moisturizer is propylene glycol.

8. An alcohol-free and paraben-free waterless shampoo composition according to claim 1, wherein the viscosity controlling agent is benzyl alcohol.

9. An alcohol-free and paraben-free waterless shampoo composition according to claim 1, wherein the skin conditioning agent is tocopherol.

10. An alcohol-free and paraben-free waterless shampoo composition according to claim 1, wherein the chelating agent is disodium EDTA.

11. An alcohol-free and paraben-free waterless shampoo composition according to claim 1, wherein the fragrance is produced by compounds that are derived from natural sources.

12. An alcohol-free and paraben-free waterless shampoo composition according to claim 1, said composition consisting of 93.59% of water.

13. An alcohol-free and paraben-free waterless shampoo composition according to claim 2, said composition consisting of 2.5% of triethanolamine lauryl sulfate.

14. An alcohol-free and paraben-free waterless shampoo composition according to claim 3, said composition consisting of 1% of cocamidopropyl betaine.

15. An alcohol-free and paraben-free waterless shampoo composition according to claim 4, said composition consisting of 0.1% of dehydroacetic acid.

16. An alcohol-free and paraben-free waterless shampoo composition according to claim 5, said composition consisting of 0.1% of benzoic acid.

17. An alcohol-free and paraben-free waterless shampoo composition according to claim 6, said composition consisting of 0.05% of sorbic acid.

18. An alcohol-free and paraben-free waterless shampoo composition according to claim 7, said composition consisting of 1.5% of propylene glycol.

19. An alcohol-free and paraben-free waterless shampoo composition according to claim 8, said composition consisting of 1% of benzyl alcohol.

20. An alcohol-free and paraben-free waterless shampoo composition according to claim 9, said composition consisting of 0.005% of tocopherol.

21. An alcohol-free and paraben-free waterless shampoo composition according to claim 10, said composition consisting of 0.05% of disodium EDTA.
, Description:FIELD OF THE INVENTION
Generally, the present disclosure relates to shampoo compositions. Particularly, it relates to waterless (dry) shampoo compositions. More particularly, it relates to alcohol-free and paraben-free waterless (dry) shampoo compositions.
BACKGROUND OF THE INVENTION
Shampooing forms an essential part of hair care in today’s society. Shampoos can broadly be classified into two types: wet shampoos and waterless (dry) shampoos.
While wet shampoos are quite efficient, they require the use of water, which is an extremely precious resource. Further, wet shampoo compositions generally contain alcohol and parabens, which may cause hair dryness and adverse health effects (depending on the concentration), respectively. Moreover, wet shampoos are often required to be used in conjunction with conditioners, which give the hair a shiny look and help in maintaining the pH balance of the hair.
Waterless shampoos (also known as dry shampoos), on the other hand, are a great way to reduce the use of water in hair maintenance. Since no water is required, waterless (dry) shampoos can be used even by people living in areas where water is scarce, including campers, backpackers, defence personnel in remote areas, and the like.
However, existing dry shampoos are largely inefficient in removing odour, dirt, sweat, and oil. Further, unlike wet shampoos, they leave behind residue that is difficult to remove. Due to these reasons, dry shampoos have not become popular with consumers.
There is therefore, a need in the art for a waterless (dry) shampoo composition that does not contain alcohol and paraben.
There is therefore, a need in the art for a waterless (dry) shampoo composition that cleans the hair completely without leaving behind any undesirable residue.
There is therefore, a need in the art for a waterless (dry) shampoo composition that can also condition the hair, thereby giving the hair a shiny look, in addition to maintaining the pH of the hair.
SUMMARY OF THE INVENTION
In order to overcome the above mentioned drawbacks, alcohol-free and paraben-free waterless (dry) shampoo compositions are disclosed, said alcohol-free and paraben-free waterless (dry) shampoo compositions consisting of 87% to 96% of water as a solvent, 1.5% to 3.5% of a primary surfactant, 0.5% to 2% of a secondary surfactant, 0.05% to 2% of a first preservative, 0.05% to 2% of a second preservative, 0.025% to 0.1% of a third preservative, 1% to 2.8% of a moisturizer, 0.5% to 2% of a viscosity controlling agent, 0.0025% to 0.01% of a skin conditioning agent, 0.025% to 0.1% of a chelating agent and 0.1% of a fragrance.
The primary surfactant is selected from the group consisting of triethanolamine lauryl sulfate, alkyl benzene sulfonates, lauric acid salts, stearic acid, alkyl ether sulfates, coconut amine oxide, dodecyl dimethyl amine oxide and N-alkyl aminoacids.
The secondary surfactant is selected from the group consisting of cocamidopropyl betaine, coco betaine, lauryl hydroxypropyl sultaine, coco hydroxypropyl sultaine, disodium cocoamphodiacetate, cocamide MEA and decyl glucoside.
The first preservative, the second preservative and the third preservative are selected from the group consisting of dehydroacetic acid, benzoic acid, sorbic acid, DMDM Hydantoin and phenoxyethanol isothiazolinone.
The moisturizer is selected from the group consisting of propylene glycol, glycerine, plant oils and panthenol.
The viscosity controlling agent is selected from the group consisting of benzyl alcohol, sodium polyaconate and tetrasodium glutamate diacetate.
The skin conditioning agent is selected from the group consisting of tocopherol and Vitamin E.
The chelating agent is selected from the group consisting of disodium EDTA, polyaspartic acid and ethylene diamine-disuccinic acid.
DETAILED DESCRIPTION OF THE INVENTION
Unless otherwise specified, all the percentages disclosed are in w/v.
Alcohol-free and paraben-free waterless (dry) shampoo compositions are disclosed, said compositions consisting of 87% to 96% of water as a solvent, 1.5% to 3.5% of a primary surfactant, 0.5% to 2% of a secondary surfactant, 0.05% to 2% of a first preservative, 0.05% to 2% of a second preservative, 0.025% to 0.1% of a third preservative, 1% to 2.8% of a moisturizer, 0.5% to 2% of a viscosity controlling agent, 0.0025% to 0.01% of a skin conditioning agent, 0.025% to 0.1% of a chelating agent and 0.1% of a fragrance.
In a preferred embodiment of the present disclosure, the solvent is water.
In an embodiment of the present disclosure, the primary surfactant is selected from the group consisting of triethanolamine lauryl sulfate, alkyl benzene sulfonates, lauric acid salts, stearic acid, alkyl ether sulfates, coconut amine oxide, dodecyl dimethyl amine oxide and N-alkyl aminoacids.
In another preferred embodiment of the present disclosure, the primary surfactant is triethanolamine lauryl sulfate.
In another embodiment of the present disclosure, the secondary surfactant is selected from the group consisting of cocamidopropyl betaine, coco betaine, lauryl hydroxypropyl sultaine, coco hydroxypropyl sultaine, disodium cocoamphodiacetate, cocamide MEA and decyl glucoside.
In yet another preferred embodiment of the present disclosure, the secondary surfactant is cocamidopropyl betaine.
In yet another embodiment of the present disclosure, the first preservative is selected from the group consisting of dehydroacetic acid, benzoic acid, sorbic acid, DMDM Hydantoin and phenoxyethanol isothiazolinone.
In yet another preferred embodiment of the present disclosure, the first preservative is dehydroacetic acid.
In yet another embodiment of the present disclosure, the second preservative is selected from the group consisting of dehydroacetic acid, benzoic acid, sorbic acid, DMDM Hydantoin and phenoxyethanol isothiazolinone.
In yet another preferred embodiment of the present disclosure, the second preservative is benzoic acid.
In yet another embodiment of the present disclosure, the third preservative is selected from the group consisting of dehydroacetic acid, benzoic acid, sorbic acid, DMDM Hydantoin and phenoxyethanol isothiazolinone.
In yet another preferred embodiment of the present disclosure, the third preservative is sorbic acid.
In yet another embodiment of the present disclosure, the moisturizer is selected from the group consisting of propylene glycol, glycerine, plant oils and panthenol.
In yet another preferred embodiment of the present disclosure, the moisturizer is propylene glycol.
In yet another embodiment of the present disclosure, the viscosity controlling agent is selected from the group consisting of benzyl alcohol, sodium polyaconate and tetrasodium glutamate diacetate.
In yet another preferred embodiment of the present disclosure, the viscosity controlling agent is benzyl alcohol.
In yet another embodiment of the present disclosure, the skin conditioning agent is selected from the group consisting of tocopherol and Vitamin E.
In yet another preferred embodiment of the present disclosure, the skin conditioning agent is tocopherol.
In yet another embodiment of the present disclosure, the chelating agent is selected from the group consisting of disodium EDTA, polyaspartic acid and ethylene diamine-disuccinic acid.
In yet another preferred embodiment of the present disclosure, the chelating agent is disodium EDTA.
The composition also contains a fragrance. The incorporation of fragrances in shampoos is well established and those skilled in the art would be able to select a suitable fragrance to achieve the desired scent.
In yet another embodiment of the present disclosure, the fragrance is a natural fragrance (fragrant compounds that are derived from natural sources).
In yet another embodiment of the present disclosure, the fragrance is a synthetically produced fragrance.
In a more preferred embodiment of the present disclosure, the disclosed alcohol-free and paraben-free waterless (dry) shampoo compositions consist of 87% to 96% of water, 1.5% to 3.5% of triethanolamine lauryl sulfate, 0.5% to 2% of cocamidopropyl betaine, 0.05% to 2% of dehydroacetic acid, 0.05% to 2% of benzoic acid, 0.025% to 0.1% of sorbic acid, 1% to 2.8% of propylene glycol, 0.5% to 2% of benzyl alcohol, 0.0025% to 0.01% of tocopherol, 0.025% to 0.1% of disodium EDTA and 0.1% of the fragrance.
In a most preferred embodiment of the present disclosure, the disclosed alcohol-free and paraben-free waterless (dry) shampoo compositions consist of 93.59% of water, 2.5% of triethanolamine lauryl sulfate, 1% of cocamidopropyl betaine, 0.1% of dehydroacetic acid, 0.1% of benzoic acid, 0.05% of sorbic acid, 1.5% of propylene glycol, 1% of benzyl alcohol, 0.005% of tocopherol, 0.05% of disodium EDTA and 0.1% of the fragrance.
The disclosed alcohol-free and paraben-free waterless (dry) shampoo compositions are to be used as given below:
1. Apply onto hair until the hair is completely wet;
2. Gently massage onto the hair;
3. Dry the hair thoroughly by wiping it with a soft towel;
4. Repeat the above steps for heavily soiled hair.
The alcohol-free and paraben-free waterless (dry) shampoo compositions disclosed herein leave behind no residue, maintain the smoothness of the hair, maintain the pH of the scalp, do not cause hair dryness, completely clean the hair by removing dirt, sweat, oil and odour, provide excellent hair conditioning and reduce the microbiological count.
The process by which the compositions are manufactured consists of mixing the primary surfactant and the secondary surfactant first in a vessel. The solvent, the first preservative, the second preservative and the third preservative are mixed in a separate vessel. The two mixtures are subsequently mixed together and cooled down. Finally, the fragrance is added.
For the examples disclosed below, the viscosity was tested using the below described procedure:
A quantity of oil (200C + 0.10) was placed in a filling tube and transferred to a capillary tube by gentle suction, taking care to prevent bubble formation in the liquid by keeping the air vent tube closed. The meniscus of the column of liquid in the capillary tube was adjusted to the level of the top graduation line. Both the vent and the capillary tubes were opened in order to permit the liquid to flow into the reservoir against atmospheric pressure. The time, in seconds, for the liquid to flow from the upper mark to the lower mark in the capillary tube was recorded.
The viscometer constant, k, was calculated from the equation:
k = v/dt
where,
v is the known viscosity of the liquid in centipoise,
d is the specific gravity of the liquid tested at 200C, and
t is the time in seconds for the liquid to pass from the upper mark to the lower mark.
Example 1:
A composition consisting of 90.4% of water, 6.2% of triethanolamine lauryl sulfate, 1% of cocamidopropyl betaine, 0.4% of citric acid and 2% of propylene glycol did not produce the required amount of foam for it to be user-friendly.
Example 2:
A composition consisting of 90.4% of water, 5% of triethanolamine lauryl sulfate, 1% of cocamidopropyl betaine, 1.2% of disodium EDTA, 0.4% of citric acid and 2% of propylene glycol produced a good amount of foam. However, the composition was found to possess a high viscosity.
Example 3:
A composition consisting of 91.4% of water, 4% of triethanolamine lauryl sulfate, 1% of cocamidopropyl betaine, 0.2% of disodium EDTA, 1% of benzyl alcohol, 0.4% of citric acid and 2% of propylene glycol produced a good amount of foam. However, the foam could not be removed without the use of water.
Example 4:
A composition consisting of 93.595% of water, 2.5% of triethanolamine lauryl sulfate, 1% of cocamidopropyl betaine, 0.05% of disodium EDTA, 1% of benzyl alcohol, 0.005% of tocopherol, 1.5% of propylene glycol, 0.1% of dehydroacetic acid, 0.1% of benzoic acid, 0.05% of sorbic acid and 0.1% of a fragrance was found to yield a fresh and clear liquid having a good viscosity.
The results of stability tests conducted on the composition disclosed in Example 4 over one month are summarized below:
Attribute Acceptable Result Initial Result Result after a month
Appearance Clean, Fresh, Clear Liquid Clean, Fresh, Clear Liquid Clean, Fresh, Clear Liquid
Viscosity About 1.22 centipoise (cps) at room temperature 1.20 cps 1.21 cps
pH at 25ºC 5.5 to 6.5 6.2 6.2
Microbial limits
• Total Aerobic microbial Count
• Total Mould and yeast count
• E.coli
• Salmonella
• Pseudomonas
NMT 100 cfu/ml
NMT 10 cfu/ml
Absent
Absent
Absent
< 21cfu/ml

< 1cfu/ml

Absent
Absent
Absent NA

The pH was determined potentiometrically by means of a glass electrode and a suitable pH meter (digital). After setting the pH meter at 25ºC, the pH meter was standardized using standard buffer solutions of pH value 6.0 and 7.0. The pH of the shampoo was then measured.
The microbial limits were determined using the below mentioned protocol.
Pre-treatment of the sample:
10 g of the preparation under examination was suspended in buffered sodium chloride- peptone solution (pH 7.0) or any other suitable medium shown to have no antimicrobial activity. The volume was adjusted to 100 ml with the same. A suitable surface active agent such as 0.1% w/v solution of Polysorbate 80 was added (where required) to assist with the suspension of poorly wettable substances.
Inactivation of antimicrobial activity: For test specimens known to contain antimicrobial substances, a corresponding inactivating agent was used to neutralize the antimicrobial activity. The inactivating agent (Polysorbate 80) was added to the chosen diluent preferably before sterilization.
All the necessary items required for the testing were kept under a laminar air flow (LAF).
The pre-sterilized petri dish was labelled with glass marker, to show the media name (soyabean casein digest agar (SCDA) for bacterial count or Sabouraud Dextrose agar (SDA) for fungal count), the name of the product, the batch number and the date of analysis.
Each of 1 ml of pre-treated sample was carefully pipetted onto previously labelled petri dish in duplicate, said petri dish being maintained under a laminar air flow.
Positive control: Known volume of cells (10-10 cells) of E.coli/ S.aureus was added in SCDA plate and allowed to solidify for 30 minutes s. Likewise, known volume of cells of Candida albicans was added in SDA plate allowed to solidify for 30 minutes.
Negative Control: SCDA/ SDA media was poured in pre-sterilized and labeled plates and allow to solidify.
The plates were incubated at respective temperatures (SCDA – 350C-370C/ SDA 200C – 250C) for 120 hours (5 days).
The incubated plates were monitored every 24 hours.
Calculation:
Average No. of colonies X Dilution factor
CFU / g = -----------------------------------------------------------
Weight of sample
It was ensured that the negative control did not show any growth at the end of the incubation period.
Pathogens test: The pathogens mainly comprise of E.coli, Salmonella, S.aureus and P.aeruginosa.
Sample preparation: 10 gm sample was aseptically transferred into sterile 90 ml SCDM broth.
The media was labelled with the media name, the product batch number and the incubation date and incubated at 300C – 350C for 18- 24 hours. After the incubation, if the media was clear, it was concluded that pathogens are absent. If turbidity was observed, then specific testing of pathogens was carried out as described below:
E.coli:
Primary test: 0.1ml of enrichment media was transferred into 10ml of MacConkey’s broth containing inverted Durham’s tube and incubated at 300C – 370C for 24 hours to 48 hours.
The tube was labelled to show enrichment transfers (SCDM to MacConkey broth), sample number and the date of enrichment and incubated at 300C – 370C for 24 hours.
After incubation, if Durhams tube showed gas and if a colour change to yellow occurred, then a loopful of the same was streaked on MacConkey agar plate and incubated for 24 – 72 hours at 300C – 370C. If no change was observed, then the testing was stopped.
Upon incubation, the plate was observed for typical culture characteristics of E.coli. If typical characteristics were found, then secondary test was conducted.
If no typical characteristics were found, the result was recorded as ‘Absent’ for E.coli.

Secondary test (Indole test):
0.5 ml kovac’s reagent was added in to pre- incubated 5 ml peptone water (1%).
After shaking, it was allowed to stand for 1 minute, the formation of a pink coloured ring was interpreted as a positive result.
The presence of acid and gas and of indole in the secondary test indicates the presence of E.coli.
Cultural characteristics of E.coli in MacConkey agar is as follows:
MacConkey agar plate Brick red, colonies may have surrounding zone of precipitated bile.

Salmonella:
0.1 ml of primary enrichment from SCDM was aseptically transferred into 10 ml of sterilized Selenite-F-Broth or 10 ml of Tetrathionate Brilliant green Broth tube.
The tube was labelled to show the enrichment transfers (SCDM to SFB/ SCDM to TTBGB), product identification and date of Enrichment and incubated at 350C – 370C for 24 hours.
After the incubation period, if the SFB tube showed turbidity and the TTBGB tubes showed disappearance of green colour with white precipitate, then loopful of enrichment was picked up and streaked on surface of pre-incubated Bismuth sulfite agar (BSA)/ Brilliant Green Agar (BGA) Media plates/ Xylose lysine Deoxycholate agar/ Deoxycholate agar plate. The plate was labelled to show enrichment transfers, (SFB to BGA/ SFB to BSA/ TTBGB to BSA) product identification and date of streaking.
Upon incubation, if the plate showed typical cultural characteristics of Salmonella, biochemical identification test was conducted to confirm the same.
Secondary test (TSI test):
Any colonies showing the typical characteristics were sub-cultured in triple sugar iron agar by first inoculating the surface of the slope with inoculating needle and then making a stab cultures with the same inoculating needle.
These two tubes were incubated at 350C – 370C for 18 - 24 hours.
After incubation, yellow butt (acidic) with pink slant (alkaline), with or without concomitant blackening of butt from H2S production in TSI tubes indicated the presence of Salmonella. The cultural characteristics of Salmonella in media plates are as follows:

Sr. No. Medium Description of colony
1 Bismuth Sulphite agar Black or green
2 Brilliant green agar Small, transparent and colourless or opaque, pinkish or white (frequently surrounded by a pink or red zone)
3 Deoxycholate citrate agar Colourless and opaque with or without black centres.
4 Xylose-lysine Deoxycholate agar Red with or without black centres.

Test for Staphylococcus aureus (S. aureus):
Upon incubation, the growth was observed in tube. Loopful of enrichment was picked up and streaked on the surface of pre- incubated Mannitol Salt agar (MSA) media plate. Finally, the plates were incubated at 350C – 370C for 24 – 48 hours.
After the incubation period, the colony morphology was observed for typical cultural characteristics of S.aureus. If typical characteristics were observed, then the presence of S.aureus was confirmed by biochemical identification test.
Secondary test: The typical colony of S.aureus was streaked from Mannitol salt agar to Baired Parker agar and incubated at 350C – 370C for 24 - 48 hours.
After Incubation, the growth was examined for black colouration. If growth showed black colouration, it was interpreted to as a positive result. Cultural characteristics of S.aureus in MSA/ Baired parker agar plates are as follows:
MSA plate Yellow colonies with yellow surrounding zone
Baired Parker agar plate Black colonies surrounded by clear zone

Test for Pseudomonas aeruginosa (P.aeruginosa):
Loopful of enriched SCDM broth was picked up and streaked on the surface of pre- incubated Cetrimide Agar (CA) media plate.
The plate was labelled to show the enrichment transfer, (SCDM to CA) product identification and date of streaking. Finally, the plate was incubated at 350C – 370C for 24 - 72 hours.
Upon examination, if none of the colonies conformed to the description given in following table, it confirmed the absence of Pseudomonas.
Medium Description of colony
Cetrimide Greenish

If any colonies conformed to the description given in above table, oxidase test was carried out to confirm the presence of Pseudomonas.
Oxidase test:
An isolated colony was spread well on oxidase disc from Cetrimide agar plate.
The production of purple colour within 5 to 10 seconds indicated a positive result.
It will be apparent to a person skilled in the art that the above description is for illustrative purposes only and should not be considered as limiting. Various modifications, additions, alterations and improvements without deviating from the spirit and the scope of the disclosure may be made by a person skilled in the art. Such modifications, additions, alterations and improvements should be construed as being within the scope of this disclosure.