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Formulation, Evaluation, and Comparison of Herbal Shampoo With Commercially Available Shampoos

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Formulation, Evaluation, and Comparison of Herbal Shampoo with


Commercially Available Shampoos

Article · October 2023


DOI: 10.22377/ajp.v17i03.4999

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ORIGINAL ARTICLE Formulation, Evaluation, and Comparison
of Herbal Shampoo with Commercially
Available Shampoos
Umesh B. Telrandhe1, Akhilesh R. Tapase1, Dilip K. Madia1,
Mahendra C. Gunde2, Naheed Waseem A. Sheikh3
1
Department of Pharmacognosy, Datta Meghe College of Pharmacy, Datta Meghe Institute of Higher Education
and Research (Deemed University), Wardha, Maharashtra, India, 2Department of Pharmacognosy, Kamla
Nehru College of Pharmacy, Butibori, Nagpur, Maharashtra, India, 3Department of Pharmacology, Hi-Tech
College of Pharmacy, Chandrapur, Maharashtra, India

Abstract

Introduction: A shampoo is essentially a detergent solution with appropriate ingredients for additional advantages
such as improved hair conditioning, lubrication, and medicine. There are many different types of shampoos on the
market today; including synthetic, herbal, medicated, and non-medicated varieties, but herbal shampoo is becoming
more and more popular among customers due to their perception that natural goods are risk-free and without
adverse effects. Aim: The aim of the present study is to formulate herbal shampoo, and evaluate and compare
its physicochemical properties with the commercially available shampoos. Materials and Methods: The herbal
shampoo was formulated by adding the extracts of Calendula officinalis, Lawsonia inermis, Citrus limonum, Citrus
ulgaric, and Santolina trifoliatus in different proportions to a 10% aqueous gelatin solution. Small amount of
methylparaben was added as a preservative and pH was adjusted with citric acid. Several quality control tests
such as physical appearance/visual inspection, pH, solid contents, foam test, viscosity test, dirt dispersion test,
surface tension, wetting test, and conditioning performance tests were performed to determine the physicochemical
properties of formulated herbal shampoo and commercial shampoos. The formulated herbal shampoo and
commercial shampoo were also evaluated for conditioning performance by blind test on twenty volunteers.
Results and Discussion: The results revealed that our formulated herbal shampoo was transparent. The results
showed good cleansing and detergency, normal pH, low surface tension, small bubble size, good viscosity, and
foam stability after 5 min. The formulated shampoo and commercial shampoos also showed comparable results for
% solid contents. The score of the conditioning performance of the tress washed with herbal shampoo was found to
be 3.2 out of 4, while the score of the commercial shampoo was 3.1 and 3.3, respectively. Conclusion: Our results
revealed that the formulated herbal shampoo has excellent conditioning performance, at par with commercially
available shampoo. However, further research and development is required to improve its quality and safety.

Key words: Commercial shampoos, cosmetics, herbal shampoo, methylparaben, physicochemical properties

INTRODUCTION sources, they are risk-free and without side effects.[2] Synthetic
surfactants are included in synthetic shampoos mainly for

I
n our daily lives, shampoos are likely the their cleansing and foaming characteristics, but lengthy
most frequently used cosmetic products
for cleaning our hair and scalp. A shampoo Address for correspondence:
is essentially a detergent solution with Mr. Umesh B. Telrandhe, Datta Meghe College
appropriate additives for additional benefits of Pharmacy, Datta Meghe Institute of Higher
such as improved hair conditioning, lubrication, Education and Research (Deemed University),
medication.[1] There are many different types of Wardha, Maharashtra, India. Phone: +91-9145500970.
shampoos available today, including synthetic, E-mail: [email protected]
herbal, medicated, and non-medicated varieties,
but consumers are becoming more and more Received: 21-07-2023
interested in herbal shampoo because they think Revised: 23-09-2023
Accepted: 30-09-2023
that because these products come from natural

Asian Journal of Pharmaceutics • Jul-Sep 2023 • 17 (3) | 544


Telrandhe, et al.: Comparative evaluation of lab based herbal shampoo with commercially available shampoos

consumption of these surfactants can produce eye and scalp saponin, sapindus acid, oleanolic, saponin A, and saponin B
irritation, hair loss, and hair dryness. We have natural herbal sesquiterpenes are all present. It can be utilized as a detergent,
shampoos as an alternative to synthetic shampoo. However, demulcent, and astringent.[9]
creating cosmetic products with entirely natural ingredients
is exceedingly challenging.[3]
MATERIALS AND METHODS
Numerous medicinal plants with possible benefits on hair
have been used for centuries in shampoo formulations Plant material
allworldwide. These therapeutic herbs can be used as extracts,
powders, crude forms, or derivatives. It is challenging to All the required plant materials were collected from the local
create a shampoo with only one natural ingredient that is market of Chandrapur (M.S) India, and some were collected
safer and softer than synthetic shampoo. It must also include from the herbal garden of Hi-Tech College of Pharmacy,
considerable foaming, detergency, and solid content, similar Chandrapur. The collected plant material was washed, dried,
to synthetic shampoo. As a result, we gave careful thought to
powdered, and stored in an airtight container for later research.
developing a pure natural cleanser employing a time-tested
method and commonly used plant material for washing hair.[4]
Extraction procedure
Herbs used in the formulation of shampoo
Powdered forms of C. officinalis, L. inermis,
Calendula officinalis L. (Marigold) C. limonum, C. ulgaric, and S. trifoliatus (100 g) were
extracted in a Soxhlet apparatus for 6 h each using distilled
C. officinalis Linn’s flower belongs to the Asteraceae family, water and ethyl acetate. To determine the yield, the extract
made up of marigolds. Flavonoids, carotenes, xanthophyll, was concentrated and weighed at reduced pressure. Table 1
and essential oils can all be found in marigold flowers. contains a list of the many extraction methods that were used
Washing painful and irritated skin with floral water is used. It to extract specific plants.
is also employed in relation to itch.[5]

Lawsonia inermis (Henna) Formulation of herbal shampoo

L. inermis belongs to the Lythraceae family is frequently used The ratios of the plant extracts were blended to create the
in cosmetology and is also referred to as henna or mehendi. shampoo, whose composition is presented in Table 2. The
The plant’s potent ability to dye is widely employed in the 10% gelatin solution was combined with herbal extracts for
beauty sector. A beloved hair color is henna. In addition, it 20 min by shaking. Furthermore, methylparaben was added
exhibits antifungal and antibacterial properties. Studies show while stirring. In the end, enough 1% citric acid solution was
that laws one, the major chemical ingredient, is responsible added to the solution to change the pH. Gelatin solution was
for its potent killing ability. The keratin of hairs and the thiol used to adjust the final volume to 100 mL.[10]
group of lawsone are tightly linked.[6]

Citrus limonum (Lemon) Evaluation of formulated herbal and commercial


shampoo
Lemon is a fruit of the Rutaceae species C. limonum.
Hesperidin, limonene, pectin, terpineol, and citral are all To evaluate the quality of commercial and prepared
found in juice. It acts as a stimulant, antibacterial agent, and formulations, several quality control tests such as physical
anti-dandruff agent.[7] appearance/visual inspection, pH, Solid contents, foam test,
viscosity test, dirt dispersion test, surface tension, wetting
Citrus vulgaris (Orange) test, and conditioning performance tests were performed.[11]
The dried or fresh epidermal component known as the orange
Physical appearance/visual inspection
peel is present in the pericarp of ripened or nearly ripe
C. ulgaric fruits belonging to the Rutaceae family. It includes The preformed herbal shampoo was evaluated for clarity,
pectin, Vitamin C, volatile oil, hesperidin, iso-hesperidin, color, odor, and foam-producing ability.[12]
and neohesperidin. Peel infusion is applied as a hair rinse.
In addition, it is employed as a carminative, flavoring, and Determination of pH
stomatic agent.[8]
The typical commercial goods were used to make a 1%
solution of the formulation, and a digital pH meter was used
Santolina trifoliatus (Reetha)
to measure the pH 200 mL of distilled water and 2 mL of
These dried fruit species S. trifoliatus belongs to the Sapindus shampoo were combined in a beaker by swirling the beaker
family are used to produce Reetha. Trifoliate II, hederagenin, rather than shaking it to get a 1% solution of shampoo.[13]

Asian Journal of Pharmaceutics • Jul-Sep 2023 • 17 (3) | 545


Telrandhe, et al.: Comparative evaluation of lab based herbal shampoo with commercially available shampoos

Table 1: Herbs and its extraction methods


S. No. Herbs Extraction
1. Calendula officinalis L. (Marigold) Distilled water was used to extract the marigold through infusion. 50 g of dried
marigold flowers were blended with 287.5 mL of boiling water in a stainless‑steel
container, covered, and left for 12 h before being drained and filtered.
2. Lawsonia inermis (Henna) Decoction was used to extract the henna. 50 g of Reetha powder were added
to 287.5 mL of water in a stainless steel container. The mixture was heated
until the distilled water was reduced to one‑fourth of the original volume, then
strained and filtered.
3. Citrus limonum Lemon) The extraction of lemon juice using boiled ethyl acetate was done using a
straightforward mechanical procedure.
4. Citrus ulgaric (Orange) Ethyl acetate was infused to extract orange peels. 287.5 mL of boiling ethyl
acetate was added to 50 g of dried orange peel in a container, which was then
covered for at least 12 h.
5. Santolina trifoliatus (Reetha) Decoction was used to extract Reetha. 287.5 mL of distilled water was added
to 50 g of Reetha powder in a stainless‑steel container before being covered.
Combination was heated until the water had reduced to a fourth of its original
volume, then strained and filtered.

Table 2: Herbal shampoo formula (for 100 mL) Foam formation = Final volume of shampoo−Initial
volume
S. Extracts of different herbs Quantity
No.
Determination of foam quality and retention
1. Marigold extract 15 mL
Test for quality and retention of foam was initiated as soon
(Calendula officinalis Linn)
as the foam formulation test result was known. Every 1 min
2. Henna extract (Lawsonia inermis) 15 mL time interval, the foam volume retention was measured.
3. Lemon juice (Citrus limonum) 15 mL
4. Orange peel extract (Citrus ulgaric) 15 mL Determination of viscosity
5. Reetha extract (Santolina trifoliatus) 15 mL The viscosity of the shampoo formulation was determined
6. Methylparaben 1 mL of 0.05% using a Brookfield viscometer (Model DV-l Plus, LV, USA)
7. Gelatin solution q.s. set at various spindle speeds ranging from 0.3 to 10 rpm. All
8. Citric acid q.s. shampoos’ viscosities were determined using the Spindle
T95 scale. Throughout the investigation, the temperature and
the size of the sample container were held unchanged.
Determination of % of solid contents
In this experiment, we first determined and recorded the Dirt dispersion test
weight of an empty, dry, clean evaporating dish. The exact Add two droplets of shampoo in a test tube to create a volume
starting weight of shampoo was determined by weighing of 10 mL. The test tube is then filled with water, one drop of
the dish after adding a sample of prepared herbal shampoo India ink, and 10 shakes. The amount of ink in the foam was
weighing about 4 g to it. The dried weight of the shampoo meticulously measured.[15]
was determined by placing the evaporating shampooing dish
on a hot plate and permitting it to entirely evaporate. The Determination of surface tension
percentage of solids was calculated using the formula shown Both surface tension for pure water and a 10% shampoo
below: solution were calculated. Since the presence of grease or
Dried weight of shampoo other lubricants significantly influenced the surface tension,
Percentage of the solids = ×100 the stalagmometer was cleaned using chromic acid and
Initial weight of shampoo
filtered water.[16]
Determination of foam formation
The following equation was used to calculate the data:
By pouring 20 mL of shampoo into a clean, dry measuring
cylinder, the initial amount of foam created by the herbal R2 = (W3−W1) N1 × R1 (W2−W1) N2
shampoo formulation was measured. The measuring cylinder was
shaken ten times to capture the final volume, and the following where,
calculations were made to determine the foam formulation.[14] W1: Beaker’s empty weight.

Asian Journal of Pharmaceutics • Jul-Sep 2023 • 17 (3) | 546


Telrandhe, et al.: Comparative evaluation of lab based herbal shampoo with commercially available shampoos

W2: Distilled water in a beaker. as a conditioning agent. A good shampoo should not flow
W3: Weight of beaker containing shampoo solution. off the hair while being used but should have enough
N1: Number of distilled water droplets. viscosity to make removal from the container easy.
N2: Number of shampoo solution drops. There are several natural substances that may be used to
R1: Distilled water’s surface tension at ambient temperature. increase viscosity. For this, we selected a 10% gelatin
R2: Shampoo solution’s surface tension. solution since it creates transparent solutions and exhibits
pseudoplastic activity. Citric acid was added to adjust the
Wetting time test pH to the desired level. Our formulated herbal shampoo
contains Lemon juice, which has natural antioxidant,
A canvas paper was cut into 1-inch diameter discs having an
chelating, and anti-dandruff properties, which also
average weight of 0.44 g. The 1% v/v shampoo solution was
maintain the acidic pH of formulation. Shampoo was
placed on the smooth surface of the disc and a stopwatch was
preserved by adding a small amount of methylparaben.
started. The time required for the disc to begin to sink was
The final formula of the prepared shampoo is presented
noted as wetting time.[17]
in Table 2.
Evaluation of conditioning performance
Evaluation of formulated herbal and commercial
The hair tress of an Indian woman was obtained from a shampoo
local salon in Chandrapur, Maharashtra. The hair tress
was cut into four swatches approximately 10 cm long and The comparative effectiveness of the formulated herbal and
around weighing 5 g. One swatch without washing served commercial shampoo was evaluated, the results of which are
as the control. The other three tresses were washed with discussed below.
the commercial and formulated herbal shampoos in an
identical manner. For each cycle, each tress was shaken Physical appearance/visual inspection
with the mixture of 10 g of a sample and 15 g of water
in a conical flask for 2 min and then rinsed with 50 mL A shampoo should seem attractive and appealing on
water. After that, each tress was left for air drying at room the outside, just like any other cosmetic product. The
temperature. The tresses were washed for a maximum physical qualities of the formulated herbal and commercial
of ten cycles. The conditioning performance of herbal- shampoos, such as color, odor, and clarity, were assessed
formulated and commercial shampoos was evaluated by a [Table 3]. Our freshly prepared herbal shampoo was clear,
blind touch test, administered to twenty randomly selected pale green, and smelled great. With the exception of color,
volunteers.[18] there was no discernible difference in odor, transparency,
or foaming properties between commercial and designed
All twenty volunteers were blindfolded and asked to touch shampoo.
and rate the four tresses for conditioning performance
from scores 1 to 4 (1 = poor; 2 = satisfactory; 3 = good; pH
4 = excellent). Because pH might irritate the eyes and skin while also being
required for healthy, luscious hair and scalp tightness, it is
Statistical analysis an essential issue in shampoo analysis.[19] Alkaline shampoos
typically allow the scalp to expand and open up, which is
The data were analyzed using analysis of variance (ANOVA). why cosmetic manufacturers sell shampoos with a broad pH
All tests were performed in triplicate and the data were range as opposed to a fixed pH value.[13]
expressed as Mean ± standard deviation. ANOVA single
factor was used for determining significance. P < 0.05 were However, new trends indicate that mildly acidic pH
considered significant. shampoos are becoming more and more well-liked by
consumers. The pH value for the prepared herbal shampoos
was 5.91 ± 0.26 as shown in Table 3 and Figure 1a, which
is near to the skin pH and its other commercially available
RESULTS AND DISCUSSION
counterparts.
Formulation of herbal shampoo
% of solids content
Herbal shampoo was formulated by mixing extracts of According to studies, shampoos with larger percentages of
C. officinalis, L. inermis, C. limonum, C. ulgaric, and solids are harder to remove from hair, whereas shampoos
S. trifoliatus in definite amounts [Table 2]. These plants with lower percentages of solids will remain fluid and be
contain a variety of phytochemicals like saponins, which removed more rapidly after use. For a balanced cleaning
have surfactants property; it also have good detergency action, an optimal shampoo should also include 20–30%
and foaming properties. S. trifoliatus extracts were added solids, according to Table 3.

Asian Journal of Pharmaceutics • Jul-Sep 2023 • 17 (3) | 547


Telrandhe, et al.: Comparative evaluation of lab based herbal shampoo with commercially available shampoos

Table 3: Physicochemical evaluation of formulated herbal and commercial shampoo


Specification Patanjali’s Reetha Dabur Vatika Prepared Herbal P‑value
shampoo shampoo shampoo
Color Black Greenish black Pale green
Transparency Transparent Transparent Transparent
Odor Pleasant Pleasant Pleasant
pH (1% solution) 6.50±0.07 7.10±0.18 5.91±0.26 <0.05*
% Solid Content 25 27 29
Foam volume 102±2.15 98±3.33 110±1.25 <0.001*
Foam type Small bubble size Small bubble size Small bubble size
Viscosity 15623 11139 10265
Dirt dispersion None Light Moderate
Surface tension (dynes/cm) 30.88 31.23 43.15 <0.05*
Wetting time (sec) 146±4.14 155±2.26 161±2.48 <0.001*
Results are mean±standard deviation (n=3); *significant difference P<0.05 by ANOVA single factor

Viscosity
The viscosity of a liquid can be thought of as its thickness. The
viscosity of a shampoo is determined by the proportion of particles
present. Our findings suggest that the viscosities of the samples
b vary progressively as the rpm increases, exhibiting pseudo plastic
activity and that all of the samples had pseudo plastic rheograms,
which is excellent for shampoo [Table 3 and Figure 1c].

Dirt dispersion
a The quantity of dirt dispersed with shampoo is an essential
factor in determining how thoroughly it cleans. Shampoos
that cause ink or dirt to concentrate in the foam are considered
low quality because they are difficult to clean and frequently
redeposited on hair.
c d e
To get better washing action, the dirt should remain in the
Figure 1: Various evaluation parameters of formulated
water component. The ink was concentrated in the water
herbal shampoo. (a) pH determination; (b) Foam quality and
portion of every shampoo, ensuring their adequate cleansing
retention; (c) Viscosity measurement; (d) Dirt dispersion test;
(e) Surface tension measurement capacity and practical usefulness.[15]

A low-quality shampoo is one that promotes the accumulation


Foam formation of ink in the foam. While dirt should stay in the water, it will
be difficult to remove any that remains in the foam. If it
Although a shampoo’s capacity to produce foam has nothing
remains in the foam, it will redeposit on the hair. According
to do with how well it cleans, it does represent the product’s
to Table 3 and Figure 1d, every shampoo sample we tested
esthetic look, making it an important evaluation factor. As
yielded favorable outcomes.
shown in Table 3, during the test, a good shampoo should
produce at least 100 cc of foam, the smaller the bubbles, the
Surface tension
longer the foam will last.
According to past studies, a perfect shampoo should be able
Foam quality and retention to reduce the surface tension of distant water from 72 dynes/
Shampoo should produce a consistent amount of foam that cm to around 40 dynes/cm.[20] As indicated in Table 3 and
lasts for at least 5 min; anything less could lead to unhappy Figure 1e, formulated herbal shampoo enhanced cleaning
customers. In our analysis, every sample displays a high and detergent qualities by lowering water’s surface tension
retention rate [Table 3 and Figure 1b]. up to 43.15 dynes/cm with P < 0.05.

Asian Journal of Pharmaceutics • Jul-Sep 2023 • 17 (3) | 548


Telrandhe, et al.: Comparative evaluation of lab based herbal shampoo with commercially available shampoos

Table 4: The mean score of the volunteers opinion on the conditioning performance of the tresses after
treatment with shampoos (n=20)
Score Patanjali’s Reetha shampoo Dabur Vatika shampoo Formulated herbal shampoo No washing
1 0 0 1 18
2 2 1 2 2
3 9 10 12 0
4 9 9 5 0
Average 3.1 3.3 3.2 1.1

Wetting time properties and is quite equivalent to those of its marketed


counterparts. It can be justified by the fact that commercial
The wetting ability of a surfactant is dependent on its
shampoo includes artificial additives including thickening
concentration. Wetting ability of surfactant is commonly
agents and surfactants, which assist in cleaning. Herbal
used to test its efficacy. The canvas disc method is a quick, shampoo that has been specially formulated exhibits favorable
efficient, and reliable test to evaluate the wetting ability physical characteristics, such as physical appearance/visual
of a shampoo.[17] The wetting time of three shampoos was inspection, pH, solid contents, foam test, viscosity test, dirt
found in the order 146 ± 4.14 < 155 ± 2.26 < 161 ± 2.48 dispersion test, surface tension, wetting test, and conditioning
for Patanjali’s Reetha shampoo, Dabur Vatika shampoo, and performance. However, further research and development is
formulated herbal shampoo, respectively. From the result, it required to improve its quality and safety.
was concluded that Patanjali Reetha shampoo contains the
maximum concentration of detergents because it had the least
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