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FORMULATION, DEVELOPMENT AND EVALUATION OF INSTANT WHITENING

FACE WASH

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 World Journal of Pharmaceutical Research
Solanki et al. SJIF Research
World Journal of Pharmaceutical Impact Factor 8.084

Volume 9, Issue 5, 2541-2557. Research Article ISSN 2277– 7105

FORMULATION, DEVELOPMENT AND EVALUATION OF INSTANT

WHITENING FACE WASH

Dnyaneshwar S. Solanki*, Prof. Suraj Dattatray Sagrule, Shrikrushna Subhash Unhale,

Quazi Bilal Ansar, Prof. M. G. Chitte and Prof. Dr. K. R. Biyani

Anuradha College of Pharmacy, Chikhli, Dist. Buldana (MS) India 443201.

ABSTRACT
Article Received on
19 March 2020,
The objective of this work is to formulate and evaluate a cosmetic
Revised on 11 April 2020, Instant Whitening Face Wash by using natural ingredient. Since the
Accepted on 01 May 2020,
ancient times, there has been awareness among people regarding the
DOI: 10.20959/wjpr20205-17516
use of plants for the essential needs of a healthy and beautiful skin.
Cosmetics are the products used to clean, beautify and promote
*Corresponding Author
attractive appearance. Cosmetics designed via incorporating natural
Dnyaneshwar S. Solanki
sources such as herbs have been proven very fulfilling, in coping up
Anuradha College of
Pharmacy, Chikhli, Dist.
with the present needs of different skin types. Skin whitening herbs is
Buldana (MS) India 443201. the practice of using substances, mixtures or physical treatments to
lighten skin colour. Skin whitening treatments work by reducing the
content of melanin of the skin. Many agents have been shown to be effective in skin
whitening. Herbs are able to modulate the metabolism of pigmentation for colour of human
skin and play a crucial protective role in skin whiteness, whereas antioxidants active in the
oxidative stress of skin aging cells may support skin health. Instant whitening face wash AF4
which was formulated showed a good rheological characteristics pH, spreadability,
stickiness, homogeneity, greater active content. Hence, this study showed that F4 was the
best formulation for instant whitening face wash. The present research has resemblance to a
skin whitening cosmetic composition containing Evodia rutaecarpa fruit extract. The instant
whitening face wash can be applied to skin, this face wash found to be very effective.
According to In-Vivo study, the product has no skin irritation after application on the skin.

KEYWORDS: Face Wash, Instant Whitening Face Wash, Evodia rutaecarpa, Melanin
Pigmentation, Antioxidants etc.

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INTRODUCTION
Face wash is the products which are used to cleanse face without drying it out. Face wash is
also commonly known as “cleanser”. Face wash product found to be equally good for all skin
type. Face wash is very helpful in removing dirt, oil and provide moisture to the dry skin.
Both face washes & cleansers are used to rid your face of dirt, oil, pollution etc. A cleanser
dissolves away excess oil makeup and grime from your face. These are oil soluble impurities.
They can be removed by a face wash too, but that might be not 100% effective. Facial skin is
the delicate and ordinary soaps can cause it to lose moisture. A face wash is a mild cleanser
that does the vital job of keeping skin clean, germ free smooth and fresh and moisturizes the
horny layer without any harshness to the skin. So that skin look young and energetic. The
purpose of face wash may be to impart cleansing, anti-wrinkle effect, anti-acne property,
moisturizing effect and fairness of skin. Skin whitening agents are believed to act on the
production and metabolism of melanin of the skin by inhibiting melanin production in
melanocytes, reducing extent of melanin. The agent which inhibit melanin production, such
as propanediol, Evodia rutaecarpa fruit extract, arbutin, kojic acid, vitamin C and its
derivatives are used in the whitening cosmetic because of their low toxicity to melanocytes.

Forms of face wash

1. Cream based face wash
2. Gel based face wash
3. Liquid based face wash
4. Face wash in powder form

Types of face wash

Generally a face wash suits all skin types however now a day different products are available
in market that are formulated to suits different skin types for example: an oily skin face wash
is made for people have oily skin conditions and does not contains oils and leaves a thin oily
film on the skin. These different types of face washes available in the market include.
1. Oily skin face wash
2. Dry skin face wash
3. Normal skin face wash

Feature of face wash

1. Removing the dead cells.
2. Rejuvenating the skin cells elevate stress.

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3. Removes oil, dirt and impurities.

4. Reduces microbial flora of skin
5. Leave skin fresh and breathing.

Gel based face wash gel

A gel is a solid jelly like material that can have properties ranging from soft and weak to hard
and tough. Gels are defined as a substantially dilute cross-linked system, which exhibits no
flow when in the steady-state. By weight, gels are mostly liquid, yet they behave like solids
due to a three-dimensional cross-linked network within the liquid. It is the cross linking
within the fluid that gives a gel its structure (hardness) and contributes to the adhesive stick
(tack). In this way gels are a dispersion of molecules of a liquid within a solid in which the
solid is the continuous phase and the liquid is the discontinuous phase. The word gel was
coined by 19th century Scottish chemist Thomas Graham by clipping from gelatin.

Skin whitening herbs

Skin whitening herbs is the practice of using substances, mixtures or physical treatments to
lighten skin colour. Skin whitening treatments work by reducing the content of melanin of the
skin. Many agents have been shown to be effective in skin whitening; some have the
beneficial effects (e.g. antioxidants, nutrients) & some are a significant risk to health (for
example, those containing mercury).

The search for natural active compounds from natural herbal medicines or Traditional
Chinese Medicines (TCMs) provides an interesting, largely unexplored area for development
of new skin-care cosmetics such as natural whitening agents like melanin biosynthesis or
tyrosinase inhibitors, which are able to modulate the metabolism of pigmentation for colour
of the human.

Skin and it play a crucial protective role in skin whiteness, whereas antioxidants active in the
oxidative stress of skin aging cells may support skin health. Melanin, which is biosynthesized
by melanocyte cells in the basal layer of the epidermis, may be over produced with chronic
sun exposure, melasma or other hyper pigmentation diseases. Therefore, whitening agents
reduce melanin over production like hyper pigmentation of darkened age spots, whereas
pigmenting agents such as melanin are designed to increase pigmentation for sun protection.
However, the inhibition of melanin biosynthesis has already been described by avoiding
ultraviolet (UV) exposure, inhibiting melanocyte metabolism and proliferation inhibiting

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tyrosinase activity or removing melanin with corneal ablation. Tyrosinase is known to be the
key enzyme in the anabolism of melanin biosynthesis in melanocytes catalyzing the initial
two steps of this pathway, including hydroxylation of tyrosine (one of monophenolic
compounds) to L-dopa (L-3,4-dihydroxyphenylalane; one of o-diphenols) and oxidation of L-
dopa to o-dopaquinone (one of o-quinones). These o-quinones are then transformed into
melanin in a series of non-enzymatic reactions. Therefore, tyrosinase inhibitors are important
constituents of cosmetics and skin whitening agents and tyrosinase becomes the key target
enzyme for screening and discovery of new inhibitory compounds. This is why a constant
search for tyrosinase inhibitors obtained by extraction from natural plants or TCMs is
underway in the hope of preventing the occurrence of this melanin over productions or hyper
pigmentation disorders. The highly reactive intermediate produced by dopa oxidation and the
reactive oxygen species (ROS) and other free radicals induced by oxidative stress in skin
cells or by UV radiation exposure have been presented to be inappropriately processed in
enhancing melanin biosynthesis, damaging DNA, probably inducing proliferation of
melanocytes. The free radicals or ROS scavengers such as antioxidants may be known to
reduce hyper pigmentation. Although the plant-derived anti-oxidants scavenge free-radicals it
is assumed that their nature and concentration vary among different kinds of plants.

However, 1, 1-diphenyl- 2 picryl hydrazyl (DPPH) is a stable radical and the DPPH free
radical-scavenging assay is a simple and widely popular method for screening free radical-
scavenging ability of compounds or antioxidant activity of plant extracts.

Uses of ingredients
As of increasing focus on skin appearance, many cosmetic and pharmaceutical companies are
focusing on research that will alter skin pigmentation. There are today many known
substances that can reduce the level of pigmentation in the skin. Many of these actives have a
tyrosinase-inhibiting effect leading to reduced total melanin production. Some of the
tyrosinase inhibitors used today is for example, kojic acid, arbutin, Evodia rutaecarpa and
different kinds of vegetal or herb extracts.

There are also molecules known to have an effect on the transfer of melanin from
melanocytes to keratinocytes, leading to an overall lighter skin colour such as nicotinamide
and soybean. Substances that increase the desquamation of the skin are also commonly used
to remove excessive melanin content within the skin, for instance retinoic acid.

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MATERIALS AND METHODS

MATERIALS
The instant whitening face wash was prepared using following chemicals, apparatus and
instruments.

Chemicals
Evodia rutaecarpa fruit extract; was purchased from BioRecurso, Parwanoo, Himachal
Predesh.
Acrypol ET- 1; was purchased from Lubrizol Ltd. Mumbai.
DmDmhydaintoin; was purchased from Subhash Chemicals, Vapi.
Triethanol amine, glycerine, ethylene di-amino acetic acid, distilled water and perfume is
available in the laboratories of college.

Apparatus
Apparatus such as beaker, glass slide, measuring cylinder, test tube, mortar pestle, volumetric
flask and sonicator apparatus are available in the laboratories of college.

Instruments
Equipments such as pH meter, mechanical stirrer, Broke field viscometer (LV viscometer),
beaker, thermometer, funnel and sonicator are available in the laboratories of college.

METHODS
Preparation of face wash base
Various formulations of batches were prepared according to the Table 1. The desired
concentration of EDTA were weighed accurately and dispersed in hot purified water (not
more than 60˚C; 50 % weight of the batch size) containing desired quantity of glycerine with
moderate stirring, then add desired quantity of Aqua SF-1 and dissolved in remaining amount
of water (50% of batch size) then, primary surfactant (Sodium Lauryl Ether Sulfate) was
added. Then, secondary surfactant (cocamidopropyl betaine) was added, then sodium
metabisulfite was added, then neutralizer Triethanolamine was added, then Preservative
(Euxyl K120) was added. This was finally mixed in formulation. Perfume was added in
sufficient quantity in all the formulations. Prepared formulations were filled in a suitable
container and labelled accordingly. These preparations were further evaluated.

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Table 1: Preparation of face wash base.

Base Formulation (BF)
Phase Contents
BF1 BF2 BF3 BF4
Water Up to 100 Up to 100 Up to 100 Up to 100
Aqua SF-1 (ml) 10 10 10 10
A
EDTA (gm) 0.1 0.1 0.1 0.1
Glycerine (ml) 5 5 5 5
Euxyl K120 (ml) 0.5 0.5 0.5 0.5
B
TEA (ml) 1.5 1.5 1.5 1.5
Sodium Metabisulfite (gm) 0.2 0.2 0.2 0.2
C SLES (ml) 16 17.5 19 20
Perfume 0.5 0.5 0.5 0.5
D CAPB (ml) 5 5.5 5.8 6
E Citric Acid q.s. q.s. q.s. q.s.

Procedure
1. Take Phase A material and mixed them until light clear solution form.
2. Take Phase B material and mixed into phase A and mix into the product up to 20 min.
3. Add Phase C material into phase A & B and mix the batch up to 20 min.
4. Add Phase D material and mixed into phase A, B and C slowly and allowed to mix batch
for 30 min.
5. Then phase E material was taken and mixed into the phase A, B, C & D and transferred
into suitable container and labeled. These preparations were further optimize and face
wash base selected.

Preparation of face wash with an active

Various formulations of batches were prepared according to the Table 2. The desired
concentration of gelling agent were weighed accurately and dispersed in hot purified water
(not more than 60˚C; 50% weight of the batch size) containing desired quantity of EDTA
with moderate stirring, avoiding air entrapment and allowed. Desired quantity of glycerine
was dissolved in remaining amount of water (50% of batch size) by gentle heating. Desired
quantity of sodium lauryl ether sulfate was added and then secondary surfactant
(cocamidopropyl betaine) was added then sodium metabisufite was added, then
triethanolamine was added, then active ingredient i.e. Evodia rutaecarpa fruit extract was
added to the above mixture. This was finally mixed with previously soaked gel formulation.
Perfume was added in sufficient quantity in all the formulations. Prepared formulations were
filled in a suitable container and labelled accordingly. These preparations were further
evaluated.

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Table 2: Preparation of face wash with an active.

Active Formulation (AF)
Phase Contents
AF1 AF2 AF3 AF4 AF4 AF4
Up to Up to Up to Up to Up to Up to
Water
100 100 100 100 100 100
A Aqua SF-1 (ml) 10 10 10 10 10 10
EDTA (gm) 0.1 0.1 0.1 0.1 0.1 0.1
Glycerine (ml) 5 5 5 5 5 5
Evodia rutaecarpa (ml) 0.15 0.15 0.15 0.15 0.15 0.15
B Euxyl K120 (ml) 0.15 0.2 0.3 0.4 0.5 0.55
TEA (ml) 1.5 1.5 1.5 1.5 1.5 1.5
Sodium metabisulfite (gm) 0.2 0.2 0.2 0.2 0.2 0.2
C SLES (ml) 20 20 20 20 20 20
Perfume 0.5 0.5 0.5 0.5 0.5 0.5
D CAPB (ml) 6 6 6 6 6 6
E Citric Acid q.s. q.s. q.s. q.s. q.s. q.s.

Procedure
1) Take Phase A material containing Aqua and Carbopol aqua SF-1, EDTA, Glycerine and
mixed them until light clear solution form.
2) Phase B material containing euxyl K120 and TEA were added and mixed into Phase A.
Allow to mix into the product up to 20 min.
3) Add Phase C material containing sodium metabisulfite solution into Phase A and B and
mixed the batch up to 20 min.
4) Add Phase D material containing CAPB into Phase A, B and C slowly and allow to mixed
batch for 30 min.
5) Then Add phase E material into phase A, B, C and D and transfer into suitable container.

EVALUATION
The prepared formulation were undergo through the In-Vitro evaluation and In-Vivo
Evaluation.

In-vitro evaluation
a) Rheological Characteristics
Rheological characteristics were studied for colour, clogging, sudden viscosity change and
feel properties.

b) Determination of pH
The PH of formulations was determined using digital pH meter. One gram of face wash was
dissolved in 100 ml of demineralised water and stored for two hours. The measurements of

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pH of each formulation were done in triplicate. Instrument was calibrated before use with
standard buffer solutions at pH 4, 7 and 9.

c) Determination of Viscosity
100 gm of each of formulation was weighed and transferred to beaker. The help of Brook
field viscometer (LV viscometer), spindle no 3 at 10 rpm for 5 min. Before measurement
declaration of face wash was done and the face wash was filled in appropriate viscosity of
formulations were determined with the Wide mouth container. Samples of the face wash were
allowed to settle over 30 min at the assay temperature (25 ±1˚C) before the measurements.
Viscosity of formulation was determined using the formula.
Viscosity (cp) = Dial Reading × Factor

d) Spreadability determination of formulations

Spreadability of formulations was determined by an apparatus suggested by Multimer et al.
which was fabricated in laboratory & used for study. The apparatus consists of a wooden
block, with a fixed glass slide with one end tied to weight pan rolled on the pulley which was
in horizontal level with fixed slide. An excess of whitening face wash sample 1.5 gm was
placed between two glass slide and a 1000 gm weight was placed on slide for 5 minutes to
between compress the sample to uniform thickness weight (60gm) was added to the pan. It
was calculated using the formula:
S = ml /t
Where,
s = spreadability in gm.cm/sec
m= weight tied to upper slide
l= length of glass slide
t= time in seconds
Length of glass slide was 11.2 cm and weight tied to upper slide was (60gm) throughout the
experiment.

e) Washability
The product was applied on hand and was observed under running water.

f) Stability study
The instant whitening face wash were also subjected to the following condition of
temperature and relative humidity during stability studies for 3 weeks at room temperature.

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g) Accelerated Stability Studies

The Face wash gel formulation was subjected to stability testing for 2 months as per ICH
Guidelines at a temperature of 40oC ± 2oC and RH 75%. The Gel formulation was analysed
for the change in appearance, pH and phytochemicals.

h) Active Drug Content

The amount of drug content was determined by taking 10 gm of containing which is
equivalent to 10 mg was added in 50 ml volumetric flask containing ethanol and mixed it well
with shaking or inverting the volumetric flask for two to three times 0.1 ml. of this solution
was diluted with 25ml fresh ethanol and active content was determined using UV
spectrophotometer at 270 nm.

In vivo evaluation
a) Skin irritation test[19]
The skin irritation was carried out on human volunteers. For formulated face wash, volunteer
were selected and 1.0 g of formulated face wash was applied on an area of two square inch to
the back of the hand. The volunteers were observed for lesions or irritation.

b) Photographic evaluation human

This was carried out on volunteer. Whitening face wash was applied on skin. The
photographs were taken before and after application of the product.

RESULTS AND DISCUSSION

Stability study of face wash base
Various base formulation batches were prepared according to the formula and these
formulations were evaluated by different tests. Based on the results best formulation was
selected for final active formulation.

Table 3: Stability study of face wash base.

Rheological characteristics
Formulation Color Consistency Viscosity Washability pH Spreadability
After 1 week at room temperature
BF1 Transparent Semisolid NC Good 6.20 5.601
BF2 Transparent Semisolid NC Good 6.40 5.401
BF3 Transparent Semisolid NC Good 6.30 5.908
BF4 Transparent Semisolid NC Good 6.50 5.410
After 2 week at room temperature
BF1 Transparent Semisolid C Good 6.80 3.501

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BF2 Transparent Liquid NC Good 6.40 5.389

BF3 Transparent Semisolid C Good 6.85 3.501
BF4 Transparent Semisolid NC Good 6.50 5.409
After 3 week at room temperature
BF1 Transparent Semisolid C Good 6.10 2.501
BF2 Transparent Liquid C Good 6.45 3.380
BF3 Transparent Semisolid C Good 6.40 3.309
BF4 Transparent Semisolid NC Good 6.50 5.408

Rheological characteristics and pH of formulation BF1 & BF2 and BF3 was found to be
sudden changes and shows spreadability and viscosity changes. These were due to high or
low concentration of gelling agent, hence these formulations were rejected and formulation
BF4 was selected for active face wash formulation.

Evaluation of Instant Whitening Face Wash

Various formulation batches of instant whitening face wash were prepared and these
formulations were evaluated by different tests. Based on the results best formulation was
selected as final formulation.

a) Rheological Characteristics
These tests include parameters such as colour, clogging, sudden viscosity change, feel.

Table 4: Rheological characteristics of instant whitening face wash.

Sudden Viscosity
Formulation Color Washability Spreadability
change
AF1 Transparent C Good 5.601
AF2 Transparent NC Good 5.401
AF3 Transparent NC Good 4.908
AF4 Transparent NC Good 5.410
AF5 Transparent C Good 5.409
AF6 Transparent C Good 5.405
F- Formulation, NC- No Change, C- Change.

Rheological characteristics of formulation AF1 found colour change. AF5 and AF6 was
found to be tacky feel and shows clogging. These was due to high concentration of gelling
agent, hence these formulation was rejected for further study.

b) Determination of pH
pH tests were performed for skin lightening gel and the results were seen as given in.

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Table 5: Determination of pH.

Parameters pH
AF2 6.2
AF3 6.3
AF4 6.5
pH of all formulations were in proper range. These formulations were used for further study.

c) Determination of Viscosity
Viscosity studies were performed for Instant Whitening Face Wash and the results were seen
as given.

Table 6: Determination of Viscosity.

Speed Factor
Spindle No. 1 Spindle No. 2 Spindle No. 3 Spindle No. 4
0.3 200 1M 4M 20M
0.6 100 500 2M 10M
1.5 40 200 800 4M
3 20 100 400 2M
6 10 50 200 1M
12 5 25 100 500
30 2 10 40 200
60 1 5 20 100

Table 7: Determination of Viscosity.

Parameters Viscosity (cp)
AF2 15200
AF3 24100
AF4 25320

Viscosity of formulations were in proper range except formulation AF2 which was found to
have low viscosity due to low concentration of gelling agent, hence was rejected for further
study.

d) Determination of Spreadability and Active Drug Content

Spreadability and Active Drug Content study were performed for instant whitening face wash
and the results were seen as given in following.

Table 8: Spreadability and Active Drug Content Determination.

Parameters Spreadability Active Drug Content (%)
AF3 5.36 ± 0.80 92.93 ± 0.50
AF4 5.40 ± 1.35 94.42 ± 0.90

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e) Stability Study
Table 9: Stability study determination of instant whitening face wash.
Formulation Color Viscosity pH Viscosity
AF3 Transparent NC 6.40 24100
AF4 Transparent NC 6.50 25320
AF3 Transparent NC 6.20 24000
AF4 Transparent NC 6.45 25250
AF3 Transparent C 6.00 23921
AF4 Transparent NC 6.40 25100
NC- No change, C- change
During stability study AF3 was more change in PH than AF4 during stability study for 3
weeks, hence AF3 formulation was rejected for further study.

In-Vivo Evaluation
a) Skin irritation study
Studies were performed for skin lightening face wash and the results were seen as given in
table.

Table 10: Skin irritation study of instant whitening face wash.

Parameters Skin irritation test
AF3 No Irritation
AF4 No Irritation

b) Photographic evaluation

Initial day After 8 days

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After 15 days

After 21 days After 30 days

Fig 1: Photographic evaluation of instant whitening face wash.

In this photographic evaluation before and after application of instant whitening face wash
was shown. These photographs indicate before application skin were not in proper texture
and after application skin were in proper texture and shows lightening effect.

CONCLUSION
Instant whitening face wash AF4 which was formulated showed a good rheological
characteristics pH, spreadability, stickiness, homogeneity, greater active content. Hence, this
study showed that F4 was the best formulation for instant whitening face wash.

The instant whitening face wash concluded that it can be applied to skin, this face wash found
to be very effective, According to In-Vivo study, the product has no skin irritation after
application on skin.

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