INTRODUCTION:

Hair is an important exoskeletal part of human body which has been associated with beauty. Hair shampoos and cleansers are used not only for cleansing purpose but also for imparting gloss to hair. Besides, shampoos should ideally ensure that hair shall retain their natural oils and stay manageable. Most importantly, their safety benefits are expected from hair products. Since, the scalp is one of the most absorbent parts of the body, the product applied to the scalp gets absorbed faster than other parts of the skin.

Synthetic shampoos have been known to have multiple side effects on hair strands, like drying out of hair, frizziness and hairfall induction. In such situations, herbal shampoos plays an important role on account of less cost and fewer side effects¹^,². Herbal shampoo can be defined as the preparation containing natural surfactants in a suitable form (liquid, powder and semisolid) which when used under appropriate conditions removes grease, dirt and debris from the scalp as well as hair shaft with no adverse effects on the hair, scalp, or health of the user.

A shampoo formulation should ideally possess the following characteristics:

· The formulation must completely and effectively remove the dust and excessive oil

· It should serve for effective hair wash.

· The shampoo should lead to the production of ample foam.

· It should get rinsed off completely.

· The formulation should leave the hair, soft, manageable and non-frizzy.

· It should impart a pleasant aroma to the hair strands.

· It should be free from side effects.

· It should be devoid of irritancy towards the skin and eye.

AIM AND SCOPE OF PRESENT WORK:

The present study was designed to combine herbal ingredients of significance in hair care as per Ayurveda. The list of ingredients for the formulations was prepared. This was followed by the literature review. The materials were collected and herbal shampoo powders were formulated. The prepared shampoo formulations were evaluated for various properties in comparison with marketed preparation and the results were tabulated.

MATERIALS AND METHODS:

1) Shikakai powder:

It is a natural hair cleansing herb that decreases hair loss and adds volume to the hair. It naturally preserves oil in hair which keeps hair healthy and lustrous. It is a great conditioning agent which imparts strength to the hair. It has been claimed to possess anti-dandruff properties.

2) Reetha powder:

It is a surfactant of herbal origin that keeps the scalp soft. It supposedly eliminates microflora that are responsible for the infections to the scalp. It nourishes hair and keeps them supple and smooth. It can be used to highlight the hair and impart natural luster to them. It is also a potential anti-dandruff agent.

3) Amla powder:

Amla has been long known to enhance hair growth and development. It enhances the hair texture and retains natural oils to accord good shine and appearance. It controls hair loss. The fatty acids in the herb conserve the moisture in the hair shaft. These fatty acids penetrate the skin, reducing dryness and dandruff. It has antioxidant properties and contributes to strengthening of the hair roots. It works as a herbal conditioner and adds bounce to limp hair.

4) Nagarmotha powder:

It has a stimulatory effect on the roots of the hair. It acts on the sebaceous gland to facilitate the development of new hair.

5) Bhringaraj:

It help in retaining the original black hair color. It also plays a role in rejuvenation of the scalp.

6) Brahmi:

It is a proven nervine tonic wherein it relieves tension stimulates and relaxes the nerves. In hair care, it helps to enhance blood circulation towards the scalp³.

7) Jatamansi:

Jatamansi is an herb which is well known to promote hair growth and for its antidandruff activity⁴.

8) Tulsi powder:

It is a fragrant, adaptogenic herb known for its healing properties. It may help prevent hair loss caused by dandruff and itching or changes in hormonal levels⁵^,⁶.

9) Fenugreek powder:

It helps in reduction of hair loss and accelerates hair growth. Fenugreek seed extract helps in improvement of hair volume. It helps to control dryness and itchiness of the scalp by eliminating dandruff ⁷.

10) Harada powder:

Harda is rich in vitamin C, iron, manganese, selenium, and copper which helps arrest the hair loss and helps in hair growth due to its Rasayana (rejuvenating) property⁸^,⁹.

11) Baheda powder:

Baheda helps in promoting dandruff control and stimulation of hair growth. This is on account of the Kashaya (astringent) and Ruksha (dry) properties of the crude drug. It helps remove excess oil and keeps the scalp dry to prevent the growth of dandruff ¹⁰^,¹¹.

12) Kapoor kachri:

Kapoor Kachri powder stimulates the roots of hair strands in order to promote hair growth. It strengthens the hair and volumizes it. It has antiseptic properties helping the skin over the scalp as well. Kapoor Kachri powder benefits in strengthening and toning the scalp and make the hair stronger and shinier¹².

13) Papaya seed powder:

Papaya exhibits positive effects on hair by helping the scalp in sebum production account of the vitamin A present in it. This aids in nourishment, strengthening, and protects the hair ¹³.

14) Rosemary:

It ensures the health of scalp and hair. Not only does it increase the blood circulation in the scalp, but it also removes excess dirt and oil, and improves the thickness of your hair¹⁴^,¹⁵.

15) Jaswand phool:

It stimulates hair growth; hibiscus contains a high amount of mucilage which acts as a conditioning agent. It treats dandruff and itchy scalp. It is known to prevent premature graying¹⁶.

Collection of ingredients:

All plant powders were obtained from Bawadekar herbal store in Kolhapur. The powders were stored in air-tight containers till the formulation stage.

Preparation of formulation:

All the required powders for the preparation of herbal shampoo powder were weighed accurately and transferred through sieve no.85 and mixed in ascending order with continuous trituration in mortar and pestle. A total of three batches of the formulation were prepared according to the weight as described in table no.1 and the formulations were labeled F1, F2, and F3. These formulations were kept in a closed containers, and a comparative study of these formulations with a marketed product was carried out¹⁷^,¹⁸.

Table no. 1: Formula for herbal shampoo powder. [40gm each]

Sr. No	Name of ingredients	F1(g)	F2(g)	F3 (g)
1	Shikakai powder	8.77	9.77	10.78
2	Reetha powder	5.45	7.45	8.45
3	Amla powder	0.79	1.79	1.79
4	Harda powder	0.78	0.289	0.289
5	Behda powder	0.78	0.289	0.289
6	Jatamansi powder	0.489	0.489	0.189
7	Kapoor kachri powder	0.489	0.489	0.189
8	Tulsi powder	0.779	0.779	0.289
9	Brahmi powder	0.779	0.779	0.289
10	Jaswand phool	0.489	0.489	0.189
11	Papaya seed powder	4.768	3.768	2.768
12	Rosemary	1.649	1.649	1.649
13	Bhringaraj powder	0.779	0.779	0.779
14	Fenugreek powder	8.768	9.768	10.768
15	Nagarmotha powder	3.768	1.768	1.768

Evaluation of herbal shampoo powder:

Organoleptic evaluation:

Organoleptic evaluation was performed for all formulations. The testing parameters were inclusive of organoleptic characteristics like colour, odour, taste, and texture. Herein, colour, texture, odour and taste were evaluated using the visual, tactile, olfactory and gustatory senses respectively.

General powder characteristics:

General powder characteristics were evaluated for parameters that could possibly affect the external properties like flow property, appearance, packaging criteria, etc. of the formulation. Characteristics evaluated under these criteria were: particle size, angle of repose, bulk density, and tapped density¹⁹^,²⁰^,²¹^,²². All three formulated shampoos and marketed shampoos were assessed for the aforementioned parameters:

Particle size:

Particle size is a parameter, which could affect various properties like spreadability, grittiness, etc. The particle size was determined by I.P. Standard sieves by mechanical shaking for 10 min.

Angle of Repose:

The angle of repose affects the flow properties of a powder. It was determined using the fix glass funnel method. A funnel was mounted at a distance of 2.5 cm above the graph paper. Powder flow was continued through the funnel till the top of the heap touches the bottom tip of the funnel. The angle of repose was calculated by applying the formula mentioned below:

θ = tan-1(h/r)

Where,

θ= Angle of repose,

r= radius of the base

h= height of the heap.

Bulk density:

Bulk density is an important characteristic for product packaging and consistency of a powdered formulation. Particle size, particle size distribution, and particle cohesiveness significantly impact the bulk density. The pre-dried powder required for measuring bulk density was filled in a 100ml graduated cylinder. Thereafter, bulk volume was determined for each of the formulated shampoo powder and the marketed shampoo powder. The bulk density was calculated by applying the formula mentioned below:

Bulk density = mass of herbal shampoo powder/ bulk volume of herbal shampoo powder.

Tapped density:

The tapped density determination involves mechanically tapping a container containing a powder sample. The initial powder volume and mass was determined using a measuring cylinder. The measuring cylinder was subjected to mechanical tapping at the rate of 100 tappings/ minute. The readings pertaining to volume or mass were recorded till changes in volume were perceptible. The tapped density was calculated by applying the formula mentioned below:

Tapped density = mass of herbal shampoo powder / tapped volume of herbal shampoo powder.

Physicochemical evaluation:

4.3.1) pH:

Determination of the pH of the herbal shampoo formulations F1, F2 and F3 was carried out at room temperature by preparing a 10% shampoo solution in distilled water using pH meter.

4.3.2) Washability:

The formulations were applied to the skin and the ease and extent of washing with water was determined through visual and tactile perception.

4.3.3) Solubility:

The ability of dissolution of a substance in a solvent is known as solubility. One gram of powder was precisely weighed and added to a beaker containing 100 ml of water. To boost the solubility, the mixture was shaken well and warmed. After cooling and filtering, the residue was weighed and recorded.

4.3.4) Skin irritation test:

This test was carried out by applying the prepared and marketed shampoo powders to the skin of the hand and then washing it with normal water after 15 minutes to see whether there are any signs of irritancy. The observations were recorded and interpreted.

Dirt dispersion:

In a big test tube containing 10 ml of distilled water, 2 g of shampoo powder was introduced. After addition of 1 drop of India ink, the test tube was stoppered and shaken 10 times. The amount of ink in the foam was estimated as none, light, moderate, or heavy²²²³.

Fig No.2: Dirt dispersion test

Extractive values:

a) Determination of Alcohol Soluble Extractive:

5g of each shampoo powder was weighed and macerated in closed flasks for twenty-four hours with 100ml of the specified strength alcohol. Frequent agitation was carried out for first six hours, following which the flasks were allowed to stand for eighteen hours.

25ml of the filtrate was evaporated to dryness in a sterile flat-bottomed shallow dish to avoid solvent loss, and then dried at 105⁰C to a consistent weight and weighed. With reference to the weight of air-dried powder, the percentage of alcohol-soluble extractive was calculated²³.

b) Determination of Water Soluble Extractive:

Chloroform water was used for determination of water soluble extractive. The procedure followed was same as that of alcohol soluble extractive. For each sample, the percentage of water-soluble extractive was calculated²³.

Ash value:

a) Determination of Total Ash:

Each air-dried shampoo powder formulation was weighed, herein, 5g from it was placed in a tared silica crucible. This was then subjected to incineration in a muffle furnace at a temperature of not more than 450⁰C until carbon was removed and the product was cooled. The overall ash percentage was computed²³.

b) Determination of Acid Insoluble Ash:

Total ash obtained was boiled for 5 minutes with 25ml of dilute hydrochloric acid and filtered. An ash less filter paper, was used to collect the insoluble matter. The insoluble matter on the filter paper was then washed with hot water and it was ignited to constant weight. The percentage of acid-insoluble ash was thereafter calculated for each sample²³.

Moisture content determination:

1.5gm of the herbal shampoo powder was placed into a flat and thin porcelain dish and then dried in an oven at 100⁰C or 105⁰C until two consecutive weighings did not differ by more than 0.5gm. The powders were cooled in a desiccator and then weighed. The loss in weight was recorded as moisture content²³.

Foaming index:

One gram of each powdered formulation was weighed accurately and transferred into a 250ml conical flask containing 100ml of boiling water. Following which, it was warmed gently for 30minutes, cooled and subjected to filtration. Using a standard volumetric flask, the volume was made up to 100ml. This extract was taken in 10 test tubes in a series of successive portions of 1, 2, 3,... 10ml and the remaining volume was made up with water to 10ml. Thus, 10 dilutions per formulation were prepared. This was followed by shaking the test tubes lengthwise for 15 seconds at the rate of 2 shakes/ second. Thereafter, the test tubes were allowed to stand for a total period of 15 minutes and the height of the foam was measured.

Following formula was applied to calculate foaming index:

Foaming index =1000/a

Where a= test tube containing the dilution in which the height of the foam= 1 cm

Marketed formulation

Fig no. 3: Determination of foaming index

Ease of rinsing:

The time taken to remove the detergent was performed by applying 5gm of shampoo, and the time taken for complete removal of frothing from wash water was determined²⁴.

Ease of combing (wet):

The ease of combing was performed by passing a comb through the wet hair and checking whether the comb glided smoothly²⁴.

Ease of combing (Dry):

The ease of combing was performed by passing a comb through the dry hair and checking whether the comb glided smoothly²⁴.

Stability study:

In accordance with ICH guidelines, the stability studies were carried out, for accelerated testing with required modifications. The prepared formulations of herbal shampoo powders i.e. F1, F2, F3 and marketed shampoo was taken and kept at room temperature (30±2⁰c) as well as at refrigerator (4±2⁰c) for a total time duration of one month. The sample were tested for their physical appearance, pH and cleansing action²⁵^,²⁶^,²⁷.

Table no. 2: Organoleptic evaluation parameters

Sr. No	Organoleptic evaluation	F1	F2	F3	Marketed formulation
1	Colour	Pale brown	Pale brown	Pale brown	Pale Brown
2	Odour	Aromatic	Aromatic	Aromatic	Aromatic
3	Taste	Characteristic	Characteristic	Characteristic	Characteristic
4	Texture	Fine smooth	Fine smooth	Fine smooth	Fine smooth

General powder characteristics:

Table no. 3: General powder characteristics

Sr. No	General powder characteristics	F1	F2	F3	Marketed formulation
1	Particle size	74.59µm	48.40µm	65.71µm	10.37µm
2	Angle of repose	35.52	35.52	39.79	33.42
3	Bulk density	0.357gm/ml	0.416gm/ml	0.384gm/ml	0.357gm/ml
4	Tapped density	0.555gm/ml	0.555gm/ml	0.625gm/ml	0.55gm/ml

Physicochemical evaluation:

Table no. 4: Physicochemical evaluation

Sr. No	Physicochemical evaluation	F1	F2	F3	Marketed formulation
1	pH	6.7	6.8	6.7	6.7
2	Washability	Easily washable	Easily washable	Easily washable	Easily washable
3	Solubility	Sparingly soluble	Sparingly soluble	Sparingly soluble	Sparingly soluble
4	Skin irritation	No harmful effect on skin	No harmful effect on skin	No harmful effect on skin	No harmful effect on skin
5	Dirt dispersion	Moderate	moderate	Moderate	Moderate
6	Extractive value a) Alcohol soluble	8.26	3.1	7.72	12.7
6	b)Water soluble	1.93	0.71	1.12	2.25
7	Ash value a) Total ash value	12	12.5	14.5	19
7	b) Acid insoluble ash	4	1.2	7	3
8	Moisture content	1.5%	1.52%	1.52%	1.58%
9	Foaming index	166.6(6ml)	142.85(7ml)	111.1(9ml)	333.3(3ml)
10	Ease of rinsing	Best	Best	Best	Best
11	Ease of combing (wet)	Better	Better	Good	Better
12	Ease of combing (dry)	Best	Best	Good	Best

Stability study:

Table no.5:- Stability evaluation parameters

Sr. No	Stability evaluation parameter	F1	F2	F3	Marketed Formulation.
1	Physical appearance- a) colour	Pale brown	Pale brown	Pale brown	Pale brown
	b) Odour	Aromatic	Aromatic	Aromatic	Aromatic
	c) Taste	Character	Character	Character	Character
2	pH	6.8	6.9	6.8	6.8
3	Cleansing action	Best	Best	good	Best

Formulation	Before	After
Marketed preparation
F1
F2
F3

MATERIALS AND METHODS:

15) Jaswand phool:

It stimulates hair growth; hibiscus contains a high amount of mucilage which acts as a conditioning agent. It treats dandruff and itchy scalp. It is known to prevent premature graying16.

It stimulates hair growth; hibiscus contains a high amount of mucilage which acts as a conditioning agent. It treats dandruff and itchy scalp. It is known to prevent premature graying¹⁶.