A Herbal Composition for Dental/ Oral Use and Process to Prepare Toothpaste Formulation Thereof

Abstract

Title: A Herbal Composition for Dental/Oral Use and Process to Prepare Toothpaste Formulation Thereof Optimized concentration of extracts of cluster fig , neem and vajradanti, taken in a ratio from 1:1:1, 1:2:1, 2;1:1 and 2:2:2, converted into toothpaste formulation using with additives like calcium carbonate as abrasive agent, sodium benzoate as preservative, glycerine as humectant, citric acid as pH regulator, honey as natural sweetener, irish moss as thickening agent, sodium laurel sulphate (SLS) as foaming agent, menthol as flavouring agent and water as vehicle, evaluated through color, odor, texture, pH, foamability, homogeneity, moisture content, abrasiveness, spreadability, viscosity, stability test and in vitro antibacterial activity confirms the stable formulation with antibacterial effects for dental/oral hygiene.

Specification

Description:Title of the Invention
"A Herbal Composition for Dental/ Oral Use and Process to Prepare Toothpaste Formulation Thereof"

Field of the Invention
The present invention relates to pharmaceutical sciences comprises of herbal composition preferably consist of extracts obtained from cluster fig, neem, and vajradanti, converted into toothpaste formulation using 'Wet Gum Method' signify antibacterial, anti-inflammatory, and astringent effects.
Background of Invention
Today's generation is important for natural products, so more and more people love to choose natural herbal products over those of chemical origin. People kept their trust in natural origin products, which we call herbal products, as they also seem very safe and effective. These herbs are mostly used for formulating various products used in everyday routine. And from the various products herbal toothpaste is one of the products. We all know about the common problems of teeth like gingivitis, inflammation, plaque, oral disease, and bad breath

Natural resources are increasingly being explored for their potential in oral hygiene specifically for dental use due to their therapeutic effects.

This research aims to explore the medicinal potential of natural plants specifically for dental use to signify their therapeutic effects, so the present invention relates to herbal composition preferably consist of extracts obtained from cluster fig, neem, and vajradanti, converted into toothpaste formulation to signify antibacterial, anti-inflammatory, and astringent effects.
Objective of Invention
The principal objective of the invention is to develop novel herbal composition preferably consist of extracts obtained from cluster fig, neem, and vajradanti converted into toothpaste formulation using wet gum method and to explore its antibacterial, anti-inflammatory, and astringent effects in dental/ oral hygiene.
The secondary objective of the invention is that the cluster fig, neem, and vajradanti extracts taken in effective concentration ratio of 1:1:1, 1:2:1, 2;1:1 and 2:2:2 converted into toothpaste with additives like calcium carbonate as abrasive agent, sodium benzoate as preservative, glycerine as humectant, citric acid as pH regulator, honey as natural sweetener, irish moss as thickening agent, sodium laurel sulphate (SLS) as foaming agent, menthol as flavouring agent and water as vehicle.
The further objective of the invention is that the prepared toothpaste formulation evaluated through color, odor, texture, pH, foamability, homogeneity, moisture content, abrasiveness, spreadability, viscosity and stability test confirms the stable formulation.
The another objective of the invention is that to the prepared toothpaste preparation evaluated for in vitro antibacterial activity confirms the antibacterial effects for dental/oral hygiene.

Summary of the Invention

The present invention relates to herbal composition preferably consist of extracts obtained from cluster fig, neem, and vajradanti, taken in effective concentration ratio of 1:1:1, 1:2:1, 2;1:1 and 2:2:2 converted into toothpaste with additives like calcium carbonate as abrasive agent, sodium benzoate as preservative, glycerine as humectant, citric acid as pH regulator, honey as natural sweetener, irish moss as thickening agent, sodium laurel sulphate (SLS) as foaming agent, menthol as flavouring agent and water as vehicle.

A herbal composition for dental/ oral use and process to prepare toothpaste formulation thereof includes: a herbal composition of cluster fig extract, neem extract and vajradanti extract in effective concentration ratio of 1:1:1, 1:2:1, 2;1:1 and 2:2:2; converted into toothpaste formulation consist of cluster fig extract from 0.5 to 2 % w/w, neem extract from 0.5 to 2 % w/w and vajradanti extract from 0.5 to 1 % w/w taken with additives includes calcium carbonate asbrasive polishing agent from 20 to 22 % w/w, sodium benzoate as preservative from 2 % w/w, glycerine as humectant from 25 % w/w , honey as natural sweetener from 5 % w/w, 1 % w/w of irish moss as thickening agent, 1 % w/w of sodium laurel sulphate (SLS) as foaming agent, 2 % w/w of citric acid as pH regulator, 0.2 % w/w of menthol as flavouring agent and water up to 100 % w/w as vehicle, herein the process to prepare toothpaste formulation includes the following steps: wherein Phase I Mixture: mixing the predetermined quantity of irish moss in hot water, previously heated at 60 oC; adding sodium benzoate slowly to said mixture; at temperature of 30 to 35 oC uniformly blending the mixture with glycerine followed by honey to form homogenous phase I mixture; Phase II mixture: powders extracts of cluster fig, neem and vajradanti in predetermined concentration uniformly mixing with calcium carbonate to form homogenous phase II mixture; Final Formulation: adding phase II mixture slowly to phase I by maintaining the temperature at 40 oC under continuous stirring and avoiding lumping to get homogenous mixture of both phases; after cooling said phase mixture, adding to it in sequential manner, predetermined quantity of menthol under continuous stirring and adjusting pH with predetermined quantity of citric acid to get final toothpaste preparation evaluated through color, odor, texture, pH, foamability, homogeneity, moisture content, abrasiveness, spreadability, viscosity, stability test and in vitro antibacterial activity confirms the stable formulation with antibacterial effects for dental/oral hygiene.

One of the preferred embodiment of the present invention is to prepare the extracts of cluster fig , neem and vajradanti, herei the powders of the crude drugs were processed and powdered extracts were prepared; taking the optimized concentration ratio of said extracts from 1:1:1, 1:2:1, 2;1:1 and 2:2:2 to be used in dental and oral hygiene as an antibacterial and anti-inflammatory preparation.

One of the preferred embodiment of the present invention that the herbal composition of cluster fig , neem and vajradanti converted into toothpaste formulation but not limited to like oral formulations using suitable additives herein mixing the predetermined quantity of irish moss in hot water, previously heated at 60 oC; adding sodium benzoate slowly to said mixture; at temperature of 30 to 35 oC uniformly blending the mixture with glycerine followed by honey to form homogenous phase I mixture; powders extracts of cluster fig, neem and vajradanti in predetermined concentration uniformly mixing with calcium carbonate to form homogenous phase II mixture; adding phase II mixture slowly to phase I by maintaining the temperature at 40 oC under continuous stirring and avoiding lumping to get homogenous mixture of both phases; then in a sequential manner, adding predetermined quantity of menthol and citric acid under continuous stirring to get final toothpaste preparation.
One of the preferred embodiment of the invention is that the toothpaste formulation evaluated through color, odor, texture, pH, foamability, homogeneity, moisture content, abrasiveness, spreadability, viscosity, stability test and in vitro antibacterial activity confirms the stable formulation with antibacterial effects for dental/oral hygiene.
Brief Description of Drawings
The following thorough explanation of the various aspects of the invention, taken in conjunction with the corresponding drawing that represents various aspects and other features of the disclosure invention.
Figure 1: Flow chart of preparation process of toothpaste formulation
Figure 2: Formulations: F1, F2, F3, and F4
Figure 3: Foaming test of formulations
Figure 4: Abrasiveness of F1 and F2 samples
Figure 5: Abrasiveness of F3 and F4 samples
Figure 6: Spreadability of formulations
Figure 7: Zone of inhibition for all four samples F1, F2, F3, and F4

Detailed Description of the Invention
The following description is of exemplary embodiments only and is not intended to limit the scope, applicability or configuration of the invention in any way. Rather, the following description provides a convenient illustration through explanation and figures for implementing exemplary embodiments of the invention. Various changes to the described embodiments may be made in the function and arrangement of the ingredients described without departing from the scope of the invention.
The use of "including", "comprising" or "having" variations thereof herein is meant to encompass the items listed thereafter and equivalents thereof as well as additional items. The terms "a" and "an" herein do not denote a limitation of quantity, but rather denote the presence of at least one of the referenced items. Further, the use of terms "first", "second", and "third", and the like, herein do not denote any order, quantity, or importance, but rather are used to distinguish one element from another.
A herbal composition for dental/ oral use and process to prepare toothpaste formulation thereof includes: a herbal composition of cluster fig extract, neem extract and vajradanti extract in effective concentration ratio of 1:1:1, 1:2:1, 2;1:1 and 2:2:2; converted into toothpaste formulation consist of cluster fig extract from 0.5 to 2 % w/w, neem extract from 0.5 to 2 % w/w and vajradanti extract from 0.5 to 1 % w/w taken with additives includes calcium carbonate asbrasive polishing agent from 20 to 22 % w/w, sodium benzoate as preservative from 2 % w/w, glycerine as humectant from 25 % w/w , honey as natural sweetener from 5 % w/w, 1 % w/w of irish moss as thickening agent, 1 % w/w of sodium laurel sulphate (SLS) as foaming agent, 2 % w/w of citric acid as pH regulator, 0.2 % w/w of menthol as flavouring agent and water up to 100 % w/w as vehicle, herein the process to prepare toothpaste formulation includes the following steps: wherein Phase I Mixture: mixing the predetermined quantity of irish moss in hot water, previously heated at 60 oC; adding sodium benzoate slowly to said mixture; at temperature of 30 to 35 oC uniformly blending the mixture with glycerine followed by honey to form homogenous phase I mixture; Phase II mixture: powders extracts of cluster fig, neem and vajradanti in predetermined concentration uniformly mixing with calcium carbonate to form homogenous phase II mixture; Final Formulation: adding phase II mixture slowly to phase I by maintaining the temperature at 40 oC under continuous stirring and avoiding lumping to get homogenous mixture of both phases; after cooling said phase mixture, adding to it in sequential manner, predetermined quantity of menthol under continuous stirring and adjusting pH with predetermined quantity of citric acid to get final toothpaste preparation evaluated through color, odor, texture, pH, foamability, homogeneity, moisture content, abrasiveness, spreadability, viscosity, stability test and in vitro antibacterial activity confirms the stable formulation with antibacterial effects for dental/oral hygiene.
Table No. 1: Formula of Herbal Composition and Tooth Paste Formulation

A) Herbal composition
Sr. No. Name of ingredient Concentration
Application
01 Cluster fig extract, Neem extract and Vajradanti extract Ratio 1:1:1, 1:2:1, 2;1:1 and 2:2:2 Anti-bacterial, Anti-bacterial and Anti-inflammatory
B) Toothpaste Formulation
Sr. No. Name of ingredient Concentration
Application
01 Cluster fig extract 0.5 to 2 % w/w Anti-bacterial
02 Neem extract 0.5 to 2 % w/w Anti-bacterial
03 Vajradanti extract 0.5 to 1 % w/w Anti-inflammatory
04 Calcium carbonate 20 to 22 % w/w Abrasives, polishing
agents
05 Sodium benzoate 2 % w/w Preservative
06 Glycerine 25 % w/w Humectant
07 Honey 5 % w/w Natural sweetener
08 Irish moss 1 % w/w Thickening agents
09 SLS 1 % w/w Foaming agent
10 Citric acid 2 % w/w pH regulator
11 Menthol 0.2 % w/w Cooling effect,
flavoring agents
12 Water up to 100 % w/w Vehicle

General procedure of preparation

A herbal composition of cluster fig extract, neem extract and vajradanti extract in effective concentration ratio of 1:1:1, 1:2:1, 2;1:1 and 2:2:2; converted into toothpaste formulation includes the following steps:

Phase I Mixture: mixing 1 % w/w of irish moss as thickening agent in hot water, previously heated at 60 oC; adding 2 % w/w sodium benzoate as preservative slowly to said mixture;

at temperature of 30 to 35 oC uniformly blending the mixture with 25 % w/w glycerine as humectant followed by 5 % w/w honey as natural sweetner to form homogenous phase I mixture;

Phase II mixture: powders extracts of cluster fig extract from 0.5 to 2 % w/w, neem extract from 0.5 to 2 % w/w and vajradanti extract from 0.5 to 1 % w/w uniformly mixing with calcium carbonate as abrasive polishing agent from 20 to 22 % w/w to form homogenous phase II mixture;

Final Formulation: adding phase II mixture slowly to phase I by maintaining the temperature at 40 oC under continuous stirring and avoiding lumping to get homogenous mixture of both phases;

after cooling said phase mixture, adding to it in sequential manner, 0.2 % w/w of menthol as flavouring agent under continuous stirring and adjusting pH with 2 % w/w of citric acid as pH regulator and adding distilled water up to 100 % w/w as vehicle to get final toothpaste preparation. (Table 1 and Figure 1)
Example 1

Toothpaste preparation

Phase I Mixture: mixing 1 % w/w of irish moss as thickening agent in hot water, previously heated at 60 oC; adding 2 % w/w sodium benzoate as preservative slowly to said mixture;

at temperature of 30 to 35 oC uniformly blending the mixture with 25 % w/w glycerine as humectant followed by 5 % w/w honey as natural sweetner to form homogenous phase I mixture;
Phase II mixture: powders extracts of cluster fig extract from 0.5 % w/w, neem extract from 0.5 % w/w and vajradanti extract from 0.5 % w/w uniformly mixing with calcium carbonate as abrasive polishing agent from 20 to 22 % w/w to form homogenous phase II mixture;
Final Formulation: adding phase II mixture slowly to phase I by maintaining the temperature at 40 oC under continuous stirring and avoiding lumping to get homogenous mixture of both phases;
after cooling said phase mixture, adding to it in sequential manner, 0.2 % w/w of menthol as flavouring agent under continuous stirring and adjusting pH with 2 % w/w of citric acid as pH regulator and adding distilled water up to 100 % w/w as vehicle to get final toothpaste preparation. (Table 1 and Figure 1)
Example 2

Toothpaste preparation

Phase I Mixture: mixing 1 % w/w of irish moss as thickening agent in hot water, previously heated at 60 oC; adding 2 % w/w sodium benzoate as preservative slowly to said mixture;
at temperature of 30 to 35 oC uniformly blending the mixture with 25 % w/w glycerine as humectant followed by 5 % w/w honey as natural sweetner to form homogenous phase I mixture;
Phase II mixture: powders extracts of cluster fig extract from 1 % w/w, neem extract from 2 % w/w and vajradanti extract from 1 % w/w uniformly mixing with calcium carbonate as abrasive polishing agent from 20 to 22 % w/w to form homogenous phase II mixture;
Final Formulation: adding phase II mixture slowly to phase I by maintaining the temperature at 40 oC under continuous stirring and avoiding lumping to get homogenous mixture of both phases;
after cooling said phase mixture, adding to it in sequential manner, 0.2 % w/w of menthol as flavouring agent under continuous stirring and adjusting pH with 2 % w/w of citric acid as pH regulator and adding distilled water up to 100 % w/w as vehicle to get final toothpaste preparation. (Table 1 and Figure 1)
Example 3

Toothpaste preparation

Phase I Mixture: mixing 1 % w/w of irish moss as thickening agent in hot water, previously heated at 60 oC; adding 2 % w/w sodium benzoate as preservative slowly to said mixture;
at temperature of 30 to 35 oC uniformly blending the mixture with 25 % w/w glycerine as humectant followed by 5 % w/w honey as natural sweetner to form homogenous phase I mixture;
Phase II mixture: powders extracts of cluster fig extract from 2 % w/w, neem extract from 1 % w/w and vajradanti extract from 1 % w/w uniformly mixing with calcium carbonate as abrasive polishing agent from 20 to 22 % w/w to form homogenous phase II mixture;
Final Formulation: adding phase II mixture slowly to phase I by maintaining the temperature at 40 oC under continuous stirring and avoiding lumping to get homogenous mixture of both phases;
after cooling said phase mixture, adding to it in sequential manner, 0.2 % w/w of menthol as flavouring agent under continuous stirring and adjusting pH with 2 % w/w of citric acid as pH regulator and adding distilled water up to 100 % w/w as vehicle to get final toothpaste preparation. (Table 1 and Figure 1)
Example 4

Toothpaste preparation

Phase I Mixture: mixing 1 % w/w of irish moss as thickening agent in hot water, previously heated at 60 oC; adding 2 % w/w sodium benzoate as preservative slowly to said mixture;
at temperature of 30 to 35 oC uniformly blending the mixture with 25 % w/w glycerine as humectant followed by 5 % w/w honey as natural sweetner to form homogenous phase I mixture;
Phase II mixture: powders extracts of cluster fig extract from 2 % w/w, neem extract from 2 % w/w and vajradanti extract from 1 % w/w uniformly mixing with calcium carbonate as abrasive polishing agent from 20 to 22 % w/w to form homogenous phase II mixture;
Final Formulation: adding phase II mixture slowly to phase I by maintaining the temperature at 40 oC under continuous stirring and avoiding lumping to get homogenous mixture of both phases;
after cooling said phase mixture, adding to it in sequential manner, 0.2 % w/w of menthol as flavouring agent under continuous stirring and adjusting pH with 2 % w/w of citric acid as pH regulator and adding distilled water up to 100 % w/w as vehicle to get final toothpaste preparation. (Table 1 and Figure 1)
Physical examination
Formulated toothpaste was evaluated under parameters of physical appearance like the following Color- The visual color of all formulations was checked. Odour- The odor of formulated toothpaste was checked by smelling the sample. Taste- Taste was checked by manually tasting a small amount of sample.
pH: For pH determination of formulated toothpaste digital pH meter was used. 10 gm of toothpaste was taken in a 150 ml beaker with 10 ml of boiled and cooled water. The suspension was formulated andpH was checked for each formulation. (pH range is 7- 9).
Foamability: 1 gm of formulated toothpaste was placed in a measuring cylinder and 10 ml of water. Closing the test tube with a stopper, the tube was shaken for 15-20 seconds and allowed to stand for 15 min. Theheight of the foam was measured.
Homogeneity: The toothpaste shall have a homogenous mass when it comes from the tube by application of normalforce at room temperature.
Moisture content: A 10-gm toothpaste sample was taken and dried in the oven at 105-degree temperature. The samplewas kept for cooling and then checked for the loss of moisture from the toothpaste by the formula mentioned below.
% moisture= Original sample weight-dry sample weight/original sample weight.
Abrasiveness: Extruded samples up to 15-20 cm long on butter paper and checked for other samples. The content was squeezed with a fingertip to check the presence of any sharp and hard particles in the toothpaste. Toothpaste should not contain any of these particles.
Spreadability: To determine the spreading ability of toothpaste samples, 1-2 gm of sample was placed between 2 glass slides, and pulled slides in opposite directions. The spreading of the toothpaste sample after 3 min was measured and an average of 3 readings was taken.
Viscosity: This is the test performed to check the thickness of the product. Viscosity is termed a fluid's resistance to flow. It is also called shear stress vs shear rate. The normal viscosity range for toothpaste ranges between 10000-50000 cP (centipoise), which is thicker than water. Viscosity affects most of the factors in the toothpaste that are spreadability, foaming, cleaning ability, and stability.
Spreadability measures how easily toothpaste spreads in the toothbrush and teeth. The toothpaste withgood viscosity maintains its consistency over time.
Here, all four samples F1, F2, F3, and F4 were tested for their viscosity after formulation. Viscositywas measured in terms of thickness. Brookfield viscometer was used for measuring viscosity.
Storage stability
Storage stability is important for toothpaste because it ensures that the toothpaste remains effective and safe for use over time. It helps maintain the right texture, color, and flavor, so it feels and tastesthe same every time you use it. Stable toothpaste also ensures that the active ingredients, like fluoride for cavity protection, stay evenly mixed and effective until you finish the tube, providing consistent benefits for oral health.
The toothpaste was filled in a tube and was kept at different temperatures like 5 degrees, room temperature, and 40 degrees to check the separation of phases among them. The storage stabilitywas performed for 45 days from the sample kept for storage stability.

Antibacterial activity
Antibacterial properties were checked by in vitro study by agar disc diffusion assay. Initially, petri plates and containers for agar making were sterilized using an autoclave for 15 minutes. The suitableagar medium was taken with bacteria like Staphylococcus aureus. Then, these cultures were placed in a Petri plate and place formulated toothpaste samples (F1-F4) over bacterial plates and incubated at 37 degrees for 24 hours. The diameter of the zone of inhibition in mm was measured using a vernier calliper. The diameter of the whole zone is measured as a zone of inhibition.
Minimum inhibitory concentrations are the smallest concentrations in which the sample gives novisible bacterial growth.
The MIC values can be determined by taking an average of readings
RESULTS & DISCUSSIONS

Preformulation studies of active ingredients
A study was done for 3 active ingredients Cluster fig extract, Vajradanti extract, and Neem extract. The color, odor, and appearance of the extract were examined. The results are mentioned in the following table.
Colour:The cluster fig extract had a yellow-brown color. The vajradanti extract appeared darkish brown-green,and the neem extract also had a darkish brown-green hue.
Odour: The cluster fig extract emitted a sweet odor. The vajradanti extract had a herbaceous scent, while theneem extract was characterized by a mild bitter odor. Appearance:
All three extracts cluster fig, vajradanti, and neem were in the form of fine powders.

Table 2. Preformulation properties of active ingredients
Property Clusterfig extract Vajradanti extract Neem extract

Color Yellow
-brown Darkish
brown- green Darkish brown-
green
Odor Sweet Herbaceous Mild bitter
Appearance Fine powder Fine powder Fine powder
Toothpaste formulation: The formulation of herbal toothpaste involves the combination of various ingredients to create products that not only clean the teeth but also promote oral health benefits. This process began with the careful selection of key ingredients and determining the appropriate proportions of each. It was crucial to ensure that the final product met safety and regulatory standards. Methodology used: A common technique used in toothpaste formulation was the wet gum method. This method involved several steps to ensure a stable and effective product. Initially, the main ingredients were mixed. These included fluoride for cavity prevention, cleaning agents like silica, foaming agents such as sodium lauryl sulfate, and humectants like glycerine. Separately, a gum mixture was prepared using gums like carrageenan and xanthan gum, which acted as thickening agents and provided a smooth texture.
The gum mixture was then gradually added to the main ingredients, resulting in a wet and sticky consistency that was essential for a uniform paste. Water or another solvent was added to hydrate the mixture, allowing the ingredients to dissolve and the gum to swell, which improved the texture and stability of the toothpaste. The mixture was thoroughly homogenized to ensure smoothness, and the pHwas adjusted to around 7 to be gentle on teeth and gums. Finally, the toothpaste underwent a final mixing to ensure all ingredients were fully incorporated, resulting in a high-quality product that effectively cleaned teeth and gums. Ingredients used
The formulation included various ingredients, each playing a specific role. For instance, cluster fig extract (0.5-2%) and neem dry extract (0.5-2%) served as anti- bacterial agents, while vajradanti dry extract (0.5-1%) acted as an anti-inflammatory. Menthol (0.2%) provided a cooling effect and served as a flavoring agent. Calcium carbonate (22%) was used as an abrasive and polishing agent, and sodium benzoate (2%) acted as a preservative. Glycerine (25%) functioned as a humectant, while citric acid or sodium hydroxide (qs) regulated thepH. Honey (5%) was added as a natural sweetener, Irish moss (1%) as a thickening agent, sodium lauryl sulfate (1%) as a foaming agent, and water (qs) as the vehicle.
The herbal toothpaste formulations involved varying concentrations of specific extracts to achieve desired therapeutic effects. In the different sample formulations labeled F1, F2, F3, and F4, the concentration of cluster fig extract, which provides anti-bacterial properties, ranged from 0.5% to 2%. For instance, F1 contained 0.5% cluster fig extract, while F4 had the highest concentration at 2%. Similarly, neem dry extract, another anti-bacterial agent, was included at 0.5% in F1, increased to 1% in both F2 and F3, and reached 2% in F4. The anti-inflammatory vajradanti dry extract was present at 0.5% in F1, increased to 0.7% in F2, andwas included at 1% in both F3 and F4. These varying concentrations allowed each formulation to potentially offer different levels of oral health benefits tailored to specific needs.
Final process:
The formulation process involved several detailed steps. In Phase 1, a batch quantity of water was heated to 60 degrees Celsius, and Irish moss was added slowly under stirring. Sodium benzoate was added and dissolved properly. Once the Irish moss was dissolved, glycerine was added when the temperature reached 30-35 degrees Celsius and stirred well. Honey was then added and stirred until ahomogenous mixture formed. In Phase 2, a batch quantity of calcium carbonate and powder extracts were added and mixed well to form a homogenous mixture.
In Step 2, the temperature of Phase 1 was maintained at up to 40 degrees Celsius, and the Phase 2 powder mixture was added to Phase 1 under fast stirring. The addition of the powder was done slowlyto prevent lumps and ensure a homogenous mixture. The mixture was stirred until it appeared homogenous. In Step 3, after forming a homogenous mixture, the batch was allowed to cool to room temperature. Menthol was added to the main mixture at room temperature and mixed under stirring. In Step 4, the pH of the formulation was checked and adjusted to the desired range using sodium hydroxide. This detailed process ensured the production of a high-quality herbal toothpaste that was effective and safe for oral health care.
Physical examination: Formulated toothpaste has to be evaluated under parameters of physical appearance like the following
Color: The visual color of the formulations F1, F2, F3, and F4 was thoroughly examined, and it was observed that all samples appeared off-white with no changes in their color. The odor of the formulated toothpaste was assessed by smelling each sample, and it was found that all samples contained menthol, which provided a menthol-like smell. This addition of menthol also contributed to a cooling sensation in the oral cavity after application.
Odor: The odor of formulated toothpaste was checked by smelling the sample. All the samples were formulated using menthol for fragrance as well as a cooling sensation in the oral cavity after application. All samples F1, F2, F3, and F4 had menthol-like smell. After applications to the oral cavity, they were able to provide a cooling sensation.
Taste:The taste was checked by manually tasting a small amount of the sample. Samples F1, F2, F3, and F4 have a mildly sweet taste due to honey. The percentage of honey was able to give moderate sweetnessin the formulation.
The below tables detailed the properties of samples F1 and F2, both of which were off- white, had a menthol-like smell, and provided a mildly sweet taste with a cooling sensation. Similarly, Table 6 showed that samples F3 and F4 shared the same off-white color, menthol-like smell, and mildly sweet taste with a cooling sensation. This consistency across different formulations confirmed the reliability and quality of the toothpaste formulations. (Figure 2)
Table 3. Organoleptic properties of F1-F2

Sr No
Title
F1
F2
1 Color Off white Off white
2 Odor Menthol like smell Menthol like smell

3
Taste Mild sweet Mild sweet

Table 4. Organoleptic properties of F3-F4


Sr .. No.
Title
F3
F4
1 Color Off white Off white

2
Odor Menthol like
smell
Menthol like smell

3
Taste Mild sweet Mild sweet
pH : Initially, the formulated toothpaste was in the acidic range. Samples F1, F2, F3, and F4 had 6.3, 6.4, 6.1, and 6.5 pH respectively. The pH was adjusted to 7.5 in the mildly basic range as the pH of the oral cavity is in a slightly basic medium. A pH was adjusted with sodium hydroxide at 7.5.
Table 5. Initial pH of formulations



Toothpaste sample
Initial pH

F1
6.3

F2
6.4

F3
6.1

F4
6.5

Foamability: The foamability results were measured for all four samples F1, F2, F3, and F4. The suspension of the toothpaste was prepared and shaken for 15-20 seconds for each sample. The foam was measured for each sample. The reading of the foam was 2.1 cm, 2.3 cm, 2.1 cm, and 2.4 cm for samples F1, F2, F3,and F4 respectively. . (Figure 3)
Table 6. Foamability of formulations


Toothpaste sample Foamability
F1 2.1 cm
F2 2.3 cm
F3 2.1 cm
F4 2.4 cm
Homogeneity: The formulated toothpaste samples F1, F2, F3, and F4 were checked for homogenous phases as they should not be separated into different phases. All four samples were checked and it was observed wasall four samples were homogenous in phase.
Moisture content: A 10-gm toothpaste sample was taken and dried in the oven at 105-degree temperature. The sample was kept for cooling and then checked for moisture loss from the toothpaste by the formula mentioned below.
% moisture= Original sample weight-dry sample weight/original sample weight.
Table 7. Moisture content of formulations

Toothpaste sample Moisture content
F1 38 %
F2 35.6%
F3 34.9%
F4 32%
Abrasiveness: Extruded samples up to 15-20 cm long on butter paper and checked for other samples. The content was squeezed with a fingertip to check the presence of any sharp and hard particles in the toothpaste.Toothpaste should not contain any of these particles.
Following are the images checked for abrasiveness of F1, F2, F3, and F4. . (Figure 4 & 5)
Spreadability: To determine the spreading ability of toothpaste samples, 1-2 gm of sample was placed between 2 glass slides, and pulled slides in opposite directions. The spreading of the toothpaste sample after 3min was measured and readings were taken. It is seen that the toothpaste which has high water content was spreading more than toothpastehaving low water content. . (Figure 6)
Table 8. Spreadability of formulations

Toothpaste sample Spreading in cm
F1 7.2 cm
F2 6.6 cm
F3 5.8 cm
F4 5.2 cm
Viscosity: Brookfield viscometer was used for measuring the viscosity of four samples F1, F2, F3, and F4. Theviscosity of all four samples F1, F2, F3, and F4 is as follows.
Table 9. Viscosity of formulations

Toothpaste sample Viscosity
F1 4100 cP
F2 3900 cp
F3 3850 cP
F4 3700 cP
Antibacterial activity: Antibacterial properties were checked by in vitro study by agar disc diffusion assay. The suitable agar medium was taken with bacteria like Staphylococcus aureus. Then, these cultures were placedin a petri plate, and formulated toothpaste samples with their suspension (F1-F4) were placed over bacterial plates and incubated at 37 degrees for 24 hours. The diameter of the zone of inhibition inmm was measured. Minimum inhibitory concentrations are the smallest concentrations in which the sample gives no visible bacterial growth.The toothpaste sample was placed in bacterial culture and incubated for 24 hours. The zone for eachsample was measured. (Figure 7)
Table 10. Zone of inhibition of formulations
Toothpaste sample Zone of inhibition
F1 8 mm
F2 10.5 mm
F3 10.3 mm
F4 11 mm
It was observed that with the increased concentration of active ingredients, the zone of inhibitions was increased, which showed that sample F4 has the best anti-microbial properties than the other three samples.
Storage stability: The toothpaste was filled in a tube and kept at different temperatures like 5 degrees, room temperature, and 40 degrees to check the separation of phases. The storage stabilitywas performed for 45 days from the sample kept for storage stability All four F1, F2, F3, and F4 samples were placed in a stability chamber at respective temperature conditions to check their stability over time. The change in texture, odor, or anyphase separation after45 days was checked.Results after storing all four samples F1, F2, F3, and F4 for 45 days can be discussed as follows:
Table 11. Stability results for F1 after storage for 45 days

Property of F1 At 5 degrees At RT At 45 degrees
Color Unchanged Unchanged Unchanged
Odor Unchanged Unchanged Unchanged
Taste Unchanged Unchanged Unchanged
pH Unchanged Unchanged Unchanged
Foamability Unchanged Unchanged Unchanged
Homogeneity Unchanged Unchanged Unchanged
Moisture content Unchanged Unchanged 40.2%
Abrasiveness Unchanged Unchanged Unchanged
Spreadability Unchanged Unchanged 8.3 cm
Viscosity Unchanged Unchanged 4300 cP
Table 12. Stability results for F2 after storage for 45 days


Property of F2 At 5 degrees At RT At 45 degrees
Color Unchanged Unchanged Unchanged
Odor Unchanged Unchanged Unchanged
Taste Unchanged Unchanged Unchanged
pH Unchanged Unchanged Unchanged
Foamability Unchanged Unchanged Unchanged
Homogeneity Unchanged Unchanged Unchanged
Moisture content Unchanged Unchanged 36%
Abrasiveness Unchanged Unchanged Unchanged
Spreadability Unchanged Unchanged 7.9 cm
Viscosity Unchanged Unchanged 4000 cP
Table 13. Stability results for F3 after storage for 45 days


Property of F3 At 5 degrees At RT At 45 degrees
Color Unchanged Unchanged Unchanged
Odor Unchanged Unchanged Unchanged
Taste Unchanged Unchanged Unchanged
pH Unchanged Unchanged Unchanged
Foamability Unchanged Unchanged Unchanged
Homogeneity Unchanged Unchanged Unchanged
Moisture content Unchanged Unchanged 35%
Abrasiveness Unchanged Unchanged Unchanged
Spreadability Unchanged Unchanged 6 cm
Viscosity Unchanged Unchanged Unchanged
Table 14. Stability results for F4 after storage for 45 days


Property of F4 At 5 degrees At RT At 45 degrees
Color Unchanged Unchanged Unchanged
Odor Unchanged Unchanged Unchanged
Taste Unchanged Unchanged Unchanged
pH Unchanged Unchanged Unchanged
Foamability Unchanged Unchanged Unchanged
Homogeneity Unchanged Unchanged Unchanged
Moisture content Unchanged Unchanged Unchanged
Abrasiveness Unchanged Unchanged Unchanged
Spreadability Unchanged Unchanged Unchanged
Viscosity Unchanged Unchanged Unchanged
The toothpaste was observed after 45 days of stability, samples F1 and F2 showed significant changes in their moisture content. It showed that if the moisture content changes then it affects its spreadabilityand viscosity at 45-degree temperature. Samples F1 and F2 showed changes in spreadability and moisture content.
Scope of the Invention
The evaluation of toothpaste samples F1 to F4 showed that all samples were consistent in color, odor, and taste F4 demonstrated the best antibacterial activity, while F3 and F4 were more stable over time compared to F1 and F2, which had noticeable changes in moisture content and viscosity after storage. Overall, F4 is the most effective and stable, making it the preferred option. It was concluded that the formulated toothpaste has anti-microbial properties against staphylococcus aureus which is the active bacteria in our oral activity. The formulation and evaluation of herbal toothpaste using multiple herbal ingredients highlight the potential of natural alternatives to conventional oral hygiene products. The incorporation of herbal ingredients enhances the antimicrobial properties of toothpaste. Proper developments and positive evaluation results of the herbal toothpaste show its efficacy in developing more and more products. In the future, research and clinical studies could get their place in the herbal market to use health-sufficient dental products, could be a promising formulation in pharmaceutical applications, in future.

It is to be understood that the present invention is not limited to the embodiments described above, it should be clear that various modifications and alterations can be made along with various features of one embodiment included in other embodiments, within the scope of the present invention.


, Claims:We claim,
1- A herbal composition for dental/oral use comprises of:
a cluster fig extract;
a neem extract;
and a vajradanti extract characterized in that an effective concentration ratio of each from 1:1:1, 1:2:1, 2;1:1 and 2:2:2 respectively, converted into toothpaste formulation effectively used in dental and oral hygiene.

2- The herbal composition for dental/oral use as claimed in claim 1 is converted into toothpaste formulation prepared through a process includes the following steps: wherein,
Phase I Mixture: mixing the predetermined quantity of irish moss in hot water, previously heated at 60 oC; adding sodium benzoate slowly to said mixture; at a temperature of 30 to 35 oC uniformly blending the mixture with glycerine with addition of honey to form homogenous phase I mixture;

Phase II mixture: powders extracts of cluster fig, neem and vajradanti in predetermined concentration uniformly mixing with calcium carbonate to form homogenous phase II mixture;

Final Formulation: adding phase II mixture slowly to phase I by maintaining the temperature at 40 oC under continuous stirring and avoiding lumping to get homogenous mixture of both phases; after cooling said phase mixture, adding to it in sequential manner, predetermined quantity of menthol under continuous stirring and adjusting pH with predetermined quantity of citric acid to get toothpaste formulation.

3- The toothpaste formulation and the process thereof as claimed in claim 1 and 2, wherein the predetermined quantities of cluster fig extract is from 0.5 to 2 % w/w, neem extract is from 0.5 to 2 % w/w and vajradanti extract is from 0.5 to 1 % w/w.

4- The toothpaste formulation and the process thereof as claimed in claim 1 and 2, wherein the predetermined quantities of the additives includes calcium carbonate as abrasive polishing agent from 20 to 22 % w/w, 2 % w/w of sodium benzoate as preservative, 25 % w/w of glycerine as humectant, 5 % w/w of honey as natural sweetener, 1 % w/w of irish moss as thickening agent, 1 % w/w of sodium laurel sulphate (SLS) as foaming agent, 2 % w/w of citric acid as pH regulator, 0.2 % w/w of menthol as flavouring agent and water up to 100 % w/w as vehicle.

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