Description:FIELD OF INVENTION
[001] The present invention relates to a waterless, alcohol free and paraben free composition for body baths, cleansers, and disinfectants. Particularly, the present invention relates to a synergistic composition comprising a combination of surfactants, antimicrobial agents, preservatives and citric acid. The composition of the present invention has antibacterial, antifungal and sporicidal properties.
BACKGROUND OF THE INVENTION
[002] Body cleansing agents such as body-baths, shampoos, tooth- pastes that provide foam-based cleaning have become integral to every household in the contemporary times. Conventionally, these cleaning agents require water for cleansing after their application. Requirement of water to rinse wet body baths make them unsuitable for use at the places with no water availability such as high altitudes, during travelling, camping or for the patients who need long-term palliative care without access to a wash basin. On the contrary, waterless body baths reduces the use of water and is suitable for use at places which face scarcity of water.
[003] Currently, a range of essential oils based waterless formulations such as waterless shampoo, waterless body wash, waterless cleanser etc. are commercially available, that produce low-foaming products. However, these cleansers primarily focus on maintaining body moisture barrier, but do not provide effective cleaning. Further, chemical based waterless cleansers are also known, however, such compositions are mostly used on the animals. There are several health issues associated with the harmful ingredients of these cleaning formulations, when used on a human body. Almost every cleanser present in the skincare market has harmful chemicals such as parabens, sodium lauryl sulfate (SLS) and alcohol as preservatives or emulsifiers. These harmful chemicals disrupt the hormonal balance, upsets the natural moisture of the skin and are carcinogenic in nature leading to breast cancer, skin cancer, eczema or abnormality of the kidneys and liver etc.
[004] Reference is made to the patent application number US20100197544A1 disclosing a body wash composition that does not require rinsing, and that topically cleanses a biological entity includes from about 0.5% to about 20.0% by weight of a concentrated extract of Arnica; and remainder pure water and the composition include a foaming agent, humectants, and/or fragrance. The prior art document specifically reduces body odour. However, the composition fails to provide protection against broad-spectrum microbes.
[005] Thus, the existing technologies fail to disclose effective cleansing compositions that are devoid of harmful chemicals and can give a long lasting antimicrobial effect and thus, aids in prevention of the spread of illness and infection in an effective manner.
[006] Therefore, there remains a need to provide an effective waterless alcohol-free and paraben-free waterless cleaning composition that is easy-to-use, safe, and hygienic and can provide cleansing effect by spraying, massaging, and wiping without leaving any undesired residue.
OBJECTIVES OF THE INVENTION
[007] The primary objective of the present invention is to provide harmful chemicals free waterless cleaning compositions.
[008] Yet another objective of the present invention is to provide alcohol free and paraben free cleaning compositions.
[009] Another objective of the present invention is to provide an effective waterless alcohol-free and paraben-free formulations such as waterless body bath, waterless body shampoo, waterless toothpaste, waterless hand wash and the like, that are easy-to-use, safe, and hygienic and which can provide cleansing effect by spraying, massaging, and wiping without leaving any residue and thus avoid the need of water to wash it off.
[010] Another objective of the present invention is to provide a synergistic composition comprising a surfactant, antimicrobial agents and citric acid.
[011] Another objective of the present invention is to provide a waterless alcohol free and paraben free composition with enhanced antimicrobial/disinfectant activity.
[012] Yet another objective of the present invention is to provide a waterless alcohol free and paraben free body cleaning composition with enhanced cleansing efficacy.
[013] Another objective of the present invention is to provide rinse free body cleansing composition with low foaming capacity and hence providing the complete body hygiene without needing water.
[014] Another objective of the present invention is to provide a highly stable waterless alcohol free and paraben free body cleaning composition with no substantial change in the chemical, physical and organoleptic characteristics for one month.
[015] Yet another objective of the present invention is to provide a non-irritant waterless alcohol free and paraben free body baths, body shampoos, hand wash, tooth paste, face cleanser and the like formulations.
[016] Yet another objective of the present invention is to provide a waterless alcohol free and paraben free composition which provides smooth skin and balances the pH of the skin.
[017] Other objects and advantages of the present invention will become apparent from the following description taken in connection with the accompanying examples to disclose the aspects of the present invention.
SUMMARY OF THE INVENTION
[018] The present invention relates to a waterless, alcohol free and paraben free cleansing compositions and formulations utilizing the said composition for use in a range of waterless products such as body bath, shampoo, hand wash, toothpaste etc. Particularly, the present invention relates to a synergistic composition comprising a primary cationic surfactant, a secondary surfactant, one or more antimicrobial/ antibacterial agents/disinfectants, preservatives, modifiers, humectants, and fragrances. The composition of the present invention has antibacterial/antimicrobial, antifungal and sporicidal properties.
DETAILED DESCRIPTION OF THE INVENTION
[019] The following is a detailed description of embodiments of the disclosure. The embodiments are in such detail as to clearly communicate the disclosure. However, the amount of detail offered is not intended to limit the anticipated variations of embodiments; on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the present disclosure.
[020] All publications herein are incorporated by reference to the same extent as if each individual publication or patent application were specifically and individually indicated to be incorporated by reference. Where a definition or use of a term in an incorporated reference is inconsistent or contrary to the definition of that term provided herein, the definition of that term provided herein applies and the definition of that term in the reference does not apply.
[021] Reference throughout this specification to "one embodiment" or "an embodiment" means that a particular feature, structure or characteristic described in connection with the embodiment is included in at least one embodiment. Thus, the appearances of the phrases "in one embodiment" or "in an embodiment" in various places throughout this specification are not necessarily all referring to the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
[022] Accordingly, those of ordinary skill in the art will recognize that various changes and modifications of the embodiments described herein can be made without departing from the scope of the invention. In addition, descriptions of well-known functions and constructions are omitted for clarity and conciseness.
[023] Features that are described and/or illustrated with respect to one embodiment may be used in the same way or in a similar way in one or more other embodiments and/or in combination with or instead of the features of the other embodiments.
[024] The terms and words used in the following description and claims are not limited to the bibliographical meanings but are merely used to enable a clear and consistent understanding of the invention. Accordingly, it should be apparent to those skilled in the art that the following description of exemplary embodiments of the present invention are provided for illustration purpose only and not for the purpose of limiting the invention.
[025] It is to be understood that the singular forms “a”, “an”, and “the” include plural referents unless the context clearly dictates otherwise.
[026] It should be emphasized that the term “comprises/comprising” when used in this specification is taken to specify the presence of stated features, integers, steps, or components but does not preclude the presence or addition of one or more other features, integers, steps, components, or groups thereof. The equations used in the specification are only for computation purpose.
[027] The present invention relates to a waterless, alcohol free and paraben free cleaning composition. Particularly, the present invention relates to a synergistic composition comprising a primary cationic surfactant, a secondary surfactant, one or more antimicrobial and/or antibacterial agents/disinfectant, preservatives, modifiers, humectants, and fragrances.
[028] The waterless composition according to present invention comprises of:
a. A primary cationic surfactant from 0.5% to 2% by weight of the total composition (wt/wt);
b. a secondary surfactant from 0.5% to 2% (wt/wt);
c. at least one antimicrobial/ antibacterial compound or disinfectant from 0.1% to 2% (wt/wt);
d. at least one humectant/moisturising agent/ antifreezing agent from 0.5% to 2% (wt/wt);
e. at least one preservative from 0.01% to 0.1% (wt/wt);
f. at least one modifier/pH controller from 0.1% to 1.0%% (wt/wt);
g. at least one fragrance from 0.001% to 2% by weight of the total composition; and
h. a solvent
[029] The primary cationic surfactant is a compound selected from capryl glucoside or caprylyl glucoside.
[030] The secondary surfactant is cocamidopropyl betaine.
[031] The preservative is a compound selected from but not limited to citric acid, benzoic acid, sorbic acid and phenoxyethanol.
[032] An antimicrobial/antibacterial agent/disinfectant is a compound selected from the group comprising of a strong base with cationic properties such as chlorhexidine digluconate, sodium benzoate, dehydroacetic acid or a combination thereof.
[033] The humectant/moisturising agent/ antifreezing agent selected from the group comprising of propylene glycol, glycerine, plant oils, lactic acid and panthenol.
[034] The modifier/pH controller selected from the group comprising of citric acid, disodium EDTA and sodium hydroxide.
[035] The fragrance selected from the group comprising of absolute repair, intense repair, lavender, rose, citrus and natural fragrance.

[036] The composition of the present invention is free from alcohol and paraben preservatives. The composition of the present invention does not require water for rinsing.
[037] The composition of the present invention may be formulated in the form of wide range of products selected from body care products such as waterless body-bath, waterless hair shampoo, waterless toothpaste, waterless soaps and handwashes, etc. or any conventional formulation, as is well known to those skilled in the art.
[038] The present invention also provides a process of preparation of the waterless bodybath composition comprising the steps of:
a. adding each ingredient in a step wise manner from the stock solution with constant stirring at 1000-2000 rpm at a temperature in the range of 20 to 25 ºC;
b. stirring the mixture obtained in step (a) for at least 20-30 minutes to completely mix all the components, so as not to have any visible residue or precipitate in the solution;
c. adjusting pH of bodybath in the range of 5.2-5.7 at room temperature by adding pH adjuster (base).
[039] In a specific embodiment, the waterless, alcohol free and paraben free composition according to embodiment of the present invention comprises:
S. No. Ingredients Composition Function Percentage
1 Propylene glycol Antifreezing agent/moisturizer/humectant 0.5% to 2.0%
2 Carpryl glucoside Primary cationic surfactant 0.5% to 2.0%
3 Cocamidopropyl betaine Secondary surfactant 0.5% to 2.0%
4 Sodium Benzoate Bacteriocide/fungicide/ antioxidant 0.1% to 2.0%
5 Citric acid Preservative/ pH controller/skin conditioning agent 0.01% to 0.1%
6 Dehydroacetic acid Bacteriocide/fungicide/ preservative 0.01% to 0.3%
7 Chlorohexidine digluconate Antimicrobial/ antiseptic 0.1% to 2.0%
8 Sodium hydroxide pH controller 0.1% to 1.0%
9 Fragrance (absolute repair) Absolute repair 0.001% to 2%
10 Water Solvent q.s. 100%

[040] The following exemplary embodiment of the present invention is provided by way of illustration and should not be construed to be limiting the scope of the present invention.
[041] In an exemplary embodiment, the waterless, alcohol free and paraben free composition according to embodiment of the present invention (EXAMPLE 1) comprises:
S. No. Ingredients Composition Function Percentage(wt/wt)
1 Propylene glycol Antifreezing agent/moisturizer 0.500%
2 Carpryl glucoside Primary cationic surfactant 1.5%
3 Cocamidopropyl betaine Secondary surfactant 1.5%
4 Sodium Benzoate Bacteriocide/fungicide/ antioxidant 0.202%
5 Citric acid Preservative/ pH controller/skin conditioning agent 0.020%
6 Dehydroacetic acid Bacteriocide/fungicide/ preservative 0.200%
7 Chlorohexidine digluconate Antimicrobial/ antiseptic 0.12%
8 Sodium hydroxide pH controller 0.707%
9 Fragrance (absolute repair) Absolute repair 0.002%
10 Water Solvent q.s. to make 100%

[042] In another exemplary embodiment, the waterless, alcohol free and paraben free composition according to embodiment of the present invention (EXAMPLE 2) comprises:
S. No. Ingredients Composition Function Percentage(wt/wt)
1 Propylene glycol Antifreezing agent/moisturizer 0.500%
2 Carpryl glucoside Primary cationic surfactant 1.010%
3 Cocamidopropyl betaine Secondary surfactant 1.100%
4 Sodium Benzoate Bacteriocide/fungicide/ antioxidant 0.202%
5 Citric acid Preservative/ pH controller/skin conditioning agent 0.020%
6 Dehydroacetic acid Bacteriocide/fungicide/ preservative 0.200%
7 Chlorohexidine digluconate Antimicrobial/ antiseptic 0.12%
8 Sodium hydroxide pH controller 0.707%
9 Fragrance (absolute repair) Absolute repair 0.002%
10 Water Solvent q.s. to make 100%

[043] Method of preparation of formulation
[044] To prepare the lab grade formulation of the body bath, each ingredient was added in a step wise manner from the stock solution with constant stirring at 1000-2000 rpm and 20-25 ºC. The beaker containing formulation was kept on stirrer for 20-30 minutes to completely mix all the components, so as not to have any visible residue or precipitate in the solution. The pH of bodybath formulation was adjusted using 10 M sodium hydroxide. The pH of bodybath formulation was found to be in the range of 5.2-5.7 at room temperature.
[045] EFFICACY OF THE COMPOSITION OF THE PRESENT INVENTION: The composition of the present invention has enhanced cleansing effect and does not leave high-level residue, can be simply wiped off with a towel/tissue without the use of water. The waterless technology has low aquatic and soil toxicity, strong biodegradability and a lower rate of bioaccumulation.
[046] The following tests were performed for determining efficacy of the composition of the present invention:
[047] Foaming Index Measurement Apparatus
[048] The Foaming indices for different compositions of body bath were determined with the help of a cylinder based apparatus. The apparatus includes 6 parallel cylinders, each with an internal diameter of about 9 cm and a height of about 29 cm and are fixed to a rotating frame occupying equivalent positions in the frame. Each cylinder is provided with a graduated scale to measure the height of the foam of the composition under investigation. These cylinders are closed at the top with the help of a removable lid, wherein the lid is provided with a 5 mm hole to allow introduction of additives (soil composition). The hole is closed with a rubber bunk, when the cylinders are subjected to rotation. The frame holding the cylinders is rotated by an electric motor that rotates the fixed cylinders along an axis perpendicular to main axis of the cylinders, such that the cylinder is cut in the middle of their length, in the plane of the frame.
[049] Compositions of body bath under investigation move or flow in the cylinder during rotation, thereby generating a turbulence that leads to the formation of foam. Cylinders were rotated at a rotation speed of about 20 rpm, by series of 10 rotations (each lasting for about 30 seconds) followed by a rest of 3 minutes between each series to allow a measure of the foam height (at the end of the 3 minutes). The foam height was determined by reading the graduated scale when the cylinders were in a vertical position after rotation:
[050] Protocol for measuring Foaming Index of the given composition:
[051] About 500 ml of composition to be investigated (maintained at 20 °C) was slowly poured into the cylinder by avoiding the formation of foam. The rotating frame holding the cylinders was rotated at a rotation speed of about 20 rotations per minute (rpm), by series of 10 rotations (each lasting for about 30 seconds) followed by a rest of 3 minutes between each series to allow a measure of the foam height (at the end of the 3 minutes).
[052] Compositions under investigation:
Table 1: Foam Height Measurement for compositions
Composition ID Composition Foam Height
1 1.01 % wt/wt of Capryl glucoside (in water) 5.0 cm
2 1.10 % wt/wt of Cocamidopropyl Betaine (in water) 7.0 cm
3 1.01 % wt/wt of Capryl glucoside (in water) + 1.10 % wt/wt of Cocamidopropyl Betaine (in water) 7.0 cm
4 0.5 % w/w of Capryl glucoside (in water) 2.2 cm
5 0.5 % w/w of Cocamidopropyl Betaine (in water) 3.1 cm
6 0.5 % w/w of Capryl glucoside (in water) + 0.5 % w/w of Cocamidopropyl betaine (in water) 5.2 cm
7 2.0 % w/w of Capryl glucoside (in water) 10.0 cm
8 2.0 % w/w of Cocamidopropyl Betaine (in water) 9.0 cm
9 2.0 % w/w of Capryl glucoside + 2.0 % w/w of Cocamidopropyl Betaine (in water) 19.0 cm
10 1.8 % w/w of Capryl glucoside (in water) 8.0 cm
11 1.8 %w/w of Cocamidopropyl Betaine (in water) 8.3 cm
12 1.8 % w/w of Capryl glucoside + 1.8% w/w of Cocamidopropyl Betaine (in water) 15 .0 cm
13 1.5 % w/w of Capryl glucoside (in water) 6.0 cm
14 1.5% w/w of Cocamidopropyl Betaine (in water) 7.0 cm
15 1.5 % w/w of Capryl glucoside (in water)+ 1.5% w/w of Cocamidopropyl Betaine (in water) 13 cm

[053] Results presented as part of the Table 1 hereinabove clearly indicate that a surfactant combination including Capryl glucoside (0.5% w/w to 2.0% w/w of the composition) and cocamidopropyl Betaine (0.5% w/w to 2.0% w/w of the composition) exhibits an exceptional synergistic behavior as compared to surprisingly low foaming index when compared to utilization thereof individually. More specifically, composition 1, i.e. 1.01 % wt/wt of Capryl glucoside (in water) + 1.10 % wt/wt of Cocamidopropyl Betaine (in water), shows a significant synergistic effect, i.e. the lowest foam height. Because the foam height is low it is easy to clean or wipe without using water for the cleaning. When the foam height of the cleansing agent increases, water is required to rinse the foam and hence maintaining the height of the foam is essential to a waterless cleanser/disinfectant.
[054] This rinse free body bath composition is engineered to provide the low foaming capacity while providing the complete body hygiene without water.
[055] In the composition 1 of the Table 1 as shown above, the mixture of 1.01 % wt/wt of Capryl glucoside (in water) + 1.10 % wt/wt of Cocamidopropyl Betaine (in water) was observed as producing low foam height in combination and which is approximately 7.0 cm, whereas the old composition producing the high foam height which is observed as 13 cm in combination of 1.5 % w/w of Capryl glucoside (in water) + 1.5% w/w of Cocamidopropyl Betaine (in water). Therefore, the novel composition of the present invention producing the synergistic effect i.e,, unexpectedly low foam height at the specific concentration and combination range i.e. 1.01 % wt/wt of Capryl glucoside (in water) + 1.10 % wt/wt of Cocamidopropyl Betaine (in water) (Table 1). Thus, foam height of 7 cm is sufficient for cleansing, which in association with the high foam maintenance time leads to better cleansing effect.
Foam Maintenance Index Measurement
[056] The Foam Maintenance index of compositions was determined with the help of a cylinder- based apparatus utilized for foaming index determination experiment.
[057] About 500 ml of composition to be investigated (maintained at 20 °C) was slowly poured into the cylinder by avoiding the formation of foam. The rotating frame holding the cylinders was rotated at a rotation speed of about 20 rotations per minute (rpm), by series of 10 rotations (each lasting for about 30 seconds) followed by a rest of 3 minutes between each series to allow a measure of the foam height (at the end of the 3 minutes).
[058] To insure the availability of foam for a given period of time to serve its purpose of cleansing; a foam maintenance test was conducted. For this, an artificial soil composition was prepared for testing the bathing soap composition effectiveness.
[059] Composition of Artificial sebum: An artificial sebum composition was used as an additive for measuring the sustainability of the foam formed in foaming index apparatus described above. Artificial sebum (including a combination of synthetic sebum and oil/clay) simulates greasy oils such as oils coming from the human skin, mixed with clay (bentonite). The weight ratio between synthetic sebum and clay was 10:4.
[060] Composition for 850 g of synthetic sebum:
[061] Table 2: Composition of Synthetic sebum
Sr. No. Ingredients Weight in gms
1 Palmitic acid 80
2 Stearic acid 40
3 Sebacic acid 45
4 Oleic acid 95
5 Linoleic acid 45
6 Paraffin wax (40-50°C) 90
7 Coconut oil (copprah) 95
8 Squalene 45
9 Mineral oil 180
10 Soja oil 45
11 Colza oil 90

[062] The above ingredients (synthetic sebum) were placed in a glass beaker and heated to a temperature of about 80°C for 15 minutes, under magnetic stirring to obtain a transparent and light coloured liquid and can be stored for several weeks as solid material after cooling. For the foam maintenance evaluations, the desired artificial sebum composition was prepared by melting about 10 g of synthetic sebum at a temperature of about 80°C followed by addition of about 4g of clay, under magnetic stirring.
[063] Foam maintenance Test:
[064] After the 10th series (of 20 rotations + 3 minutes resting times), artificial sebum addition was effected by adding 5 droplets (about 0.15 g) of liquid and warm oil (80°C) into the cylinder. The cylinder was given 10 subsequent rotations at 20 rpm. The foam height was measured 3 minutes after the 10 rotations (total of 200+10=210 rotations). The addition of the artificial sebum was repeated. The addition of the artificial sebum was done just after the foam height measure and just before the subsequent rotation. This rotation was measured and artificial sebum addition implement was repeated, until the foam height reached a value of about 1.6 cm. Foam Maintenance Time (in seconds) required for foam to subside (i.e. decrease in height of foam) from initial 1.6 cm to 1.0 cm was measured in seconds. More time required to subside the foam indicates the stability of the composition to effectively clean the oil/dirt that is needed to be cleaned from the human skin.
[065] Table 3: Foam Maintenance Time (in seconds) for compositions
Composition
ID Composition Foam Maintenance Time (Seconds)
1. 0.5 % w/w of Capryl glucoside (in water) + 0.5 % w/w of Cocamidopropyl betaine (in water) 78
2. 1.01 % wt/wt of Capryl glucoside (in water) + 1.10 % wt/wt of Cocamidopropyl Betaine (in water) 114
3. 1.5 % wt/wt of Capryl glucoside
(in water) + 1.5% wt/wt of Cocamidopropyl Betaine (in water) 88
4. 1.8 % w/w of Capryl glucoside + 1.8% w/w of Cocamidopropyl Betaine (in water) 98
5. 2.0 % w/w of Capryl glucoside + 2.0 % w/w of Cocamidopropyl Betaine (in water) 96
6. Composition as prepared in Example 2 115
7. Composition as Example 1 89

[066] Results presented as part of the Table 1 and Table 3 hereinabove clearly indicate that a surfactant combination including capryl glucoside (0.5 % to 2.0 % by wt. of the composition) and cocamidopropyl betaine (0.5 % to 2.0 % by wt. of the composition) exhibits an exceptional synergistic behaviour in terms of surprisingly low foaming index(i.e. measure of height of the foam produced by the equivalent of 1 g of composition under the stated test conditions) and high foam maintenance time (i.e. more cleansing effect), when compared to utilization thereof individually, while retaining its cleaning efficacy. Accordingly, the surfactant combination of the present invention is found to be of specific utility in the rinse-free body bath compositions.
[067] Specifically, the composition 1.01 % wt/wt of Capryl glucoside (in water) + 1.10 % wt/wt of Cocamidopropyl Betaine (in water) shows high foam maintenance time of 114 second in comparison to other combinations as mentioned in the Table 3. This synergistic effect significantly increases the foam density of the product at the specified concentration as shown in example 2, whereas the foam maintenance time significantly decreases at other combination (see Table 1), in the previous formulation the combination of 1.5 % wt/wt of Capryl glucoside (in water) + 1.5% wt/wt of Cocamidopropyl Betaine (in water) providing low foam height maintenance time which is approximately 88 cm in comparison to the new composition i.e. 114 cm.
[068] Anti-microbial activity of the composition
[069] The composition of Example 1 was tested for its anti-microbial activity by a time kill assay. The assay notes the changes in the microbial population within a specified time in presence of the composition. The time kill assays were performed on the ready-to-use formulation. The assays were performed as per the American Standard for Testing and Material protocol ASTM-E2315-16.
[070] TEST PROCEDURE- The working cultures of the test organisms were prepared. 10 mL of the sample was taken with respect to individual test culture. 100 µL of adjusted test cultures were inoculated in individual samples prepared. A contact time of 20-60 seconds was considered. Using the pour plate technique 1 mL of the formulation was pipetted to triplicated petri dishes for each dilution prepared by serial dilution technique and then 20mL of melted SCDA was added. The petri dish was incubated at 30-35 °C for 72 hours. The colonies on the petri dishes were counted with the help of colony counter after incubation and the observations were recorded in cfu (colony forming unit). The petri dish showing a number of colonies included in a 15-300 for bacterial and fungal of 15-150 range was used to perform the result calculation.
[071] LOG REDUCTION CALCULATION: The effectiveness of the disinfection procedure against each challenge organism was calculated for each product as a log10 reduction as follows:
[072] Log10 Reduction per product = Log10 [Positive Control Count] – Log10 [Test Surface Count]
[073] (The log reduction was rounded to the nearest 0.1 value). For each product concentration and each experimental condition, calculated and recorded the decimal log reduction separately.
[074] ACCEPTANCE CRITERIA: In case of surface challenge test positive control should yield 50 to 200% recovery of the microorganism in comparison to inoculums added. Bactericidal, fungicidal or yeasticidal activity on surfaces for general purposes is characterized by the concentration of the tested product. Agents should demonstrate a 3 log reduction of vegetative test organisms and mold spores.
[075] Results: The results of the test are provided in Table 4 as depicted below:
[076] Table 4: Anti-microbial activity of the composition of Example 1
S. No. Organism Contact time
% reduction
1 Candida L albicans(MTCC 227) 30 Sec 99.93%
1 Min 100.00%
5 Min 100.00%
2 S. aureus (ATCC 6538) 30 Sec 99.92%
1 Min 100.00%
5 Min 100.00%
3 Staph. Epidermis (ATCC12228) 30 Sec 99.98%
1 Min 100.00%
5 Min 100.00%
4 Escherichia coli (ATCC 8739) 30 Sec 99.99%
1 Min 100.00%
5 Min 100.00%
6 Aspergillus brasilensis (ATCC16404) 30 Sec 99.95%
1 Min 100.00%
5 Min 100.00%
7 P.acnes (MTCC 1951) 30 Sec 99.98%
1 Min 100.00%
5 Min 100.00%

[077] The above results clearly indicate that the composition of the present invention provides quick action as the anti-microbial efficacy was about 99.9% within 30 seconds of use. Additionally, the composition shows broad spectrum activity with triple action antibacterial, antifungal, and sporicidal.
[078] Evaluation of synergy of antimicrobial activity
[079] Disk-diffusion test: The disinfectant activity was evaluated by Disk diffusion test. In this study, a disk diffusion test was performed on Staph. Epidermis (ATCC12228) using the composition of Example 2 and some comparative compositions as shown in Table 5.
[080] Table 5: Disk-diffusion tests
S. No Component Antimicrobial Inhibition Zone (cm)
COMPOSITION
1. Chlorohexidine Digluconate (0.12%) 3.0
2. Chlorohexidine Digluconate (0.12%) + Dehydroacetic Acid (0.2 %) 3.0
3. Chlorohexidine Digluconate (0.12%) + Citric Acid (0.02 %) 3.0
4. Chlorohexidine Digluconate (0.12%) +Dehydroacetic Acid (0.2%) + Citric Acid (0.02%) 4.8
5. Formulation as in Example 2 4.8

[081] It was concluded from the results that disinfectant activity of chlorohexidine digluconate was significantly increased by addition of dehydroacetic acid and citric acid in the specific weight percentage ranges and the composition shows synergistic effect. However, there was no increase in antimicrobial inhibition zone upon addition of dehydroacetic acid only and similarly for citric acid, whereas in combination of chlorohexidine digluconate, citric acid, and dehydroacetic acid, the antimicrobial/disinfectant activity increased significantly as shown in table 5. Therefore, it can be concluded that the activity of chlorohexidine digluconate accelerated in the presence of citric acid and dehydroacetic acid, and hence mutually regulated.
[082] The antimicrobial activity of the Clensta body bath lab grade (BBL), industrial grade (BBI), and pure 0.12 % chlorhexidine (C) was observed against skin, impure water, and soil samples (Fig 3). It was found that BBL, BBI, and C shows good antimicrobial inhibition zone against all the tested samples. It was also found that extend of inhibition zone depends upon concentration of body bath and also on the underlying bacterial fixation.
[083] Cleansing activity
[084] The cleansing efficacy of the waterless body bath was measured physically with visual examination. To perform this test an ample amount of grease was applied on clean and dry hands of nine to ten volunteers (Fig 2). In that case, one hand was considered as control to see the difference after using the product (Fig 2). In second hand waterless body bath was sprayed to physically remove the grease stain. The body bath was sprayed, massaged for forty-five seconds and then wiped out using a clean tissue or towel. This experiment was carried out with four different stains such as vehicle grease, dirt/mud, lipstick and ink and it was observed that the stain of grease, dirt/mud and lipstick (seen inside the area marked by the permanent marker) were completely removed by waterless body bath. The area of application was found smooth and soft after the application.
[085] Dirt dispersion test
[086] Dirt dispersion test was carried out as per the protocol mentioned in SOP No. CL1.9.1. In this method, sample was prepared by adding one drop of India ink to 200 µL volume of waterless body bath and further the sample volume was made up to 10 mL using distilled water. This dirt dispersion experiments were carried out for body bath (lab and industrial grade) and compared with commercial grade body bath.
Table 6: Dirt dispersion ability of waterless body bath
S. No. Sample Foaming (cm) Ink Inspection
1 SLS(control) 3.4 High
2 Waterless body bath (manufacturing) 3.2 Moderate
3 Waterless body bath (lab) 3.2 Moderate

[087] The falcon tube containing the sample was vortexed at 2000 rpm for 3-5 minutes. In case of body bath samples according to the present invention (industrial and lab grade), amount of ink in the foam was observed as moderate, whereas in case of commercial grade body bath amount of ink was found to be high (Figure 1 & Table 6). This result indicates that dirt dispersion potency of body bath products manufactured in the lab and industry was good in comparison to that of commercial grade body bath. It has been well established that formulation which causes the ink to concentrate in the foam are considered of poor quality because ink or dirt that stays in foam is difficult to rinse away and gets re-deposited. Therefore, the dirt should stay in the water portion for achieving better cleansing action.
[088] Stability Test
[089] The immediate preliminary stability testing (Centrifugation test, Freeze defrost cycle, and Thermal stress) of the body bath was performed to obtain the various stability parameters of the body bath. To prepare the formulation, all the ingredients were dissolved separately and then mixed in a stepwise manner. The samples were degassed to measure the PDI and viscosity values of the various formulations.
[090] pH value of the body bath formulation was determined using a digital pH meter (EuTech pH 510). pH determination test was carried out as per the protocol mentioned in SOP No. CL1.0.The pH value was measured at three days of interval for 30 days in triplet samples at room temperature. The pH value of the body bath formulation was found to be in the range of pH 5.2-6.0 (Table 7) with no recorded change from 0 to 30 days of incubation. It generally indicates acidic nature of the body bath is good for removing the dirt, dust and oil from the skin. Next, pH value of the body bath formulation was monitored at various stress conditions and it was found that pH value was consistent for up to 30 days without any significant change (Table 8, 9 and 10).
[091] Visual inspection/physical appearance
[092] Organoleptic characteristics of the body bath formulations were monitored macroscopically and technically in terms of their odor, smell, clarity, and foaming ability.
[093] The result of visual inspection of the body bath formulation is shown in Table 7. It was also observed that body bath formulation is stable for up to 30 days at various stress conditions and showed similar organoleptic characteristics with respect to the complete formulation at zero day. It was also found that the complete formulation does not show any significant changes in their physical appearance from 0 to 30 days at different stress conditions (Table 8, 9, and 10).
[094] Viscosity measurement
[095] The viscosity of the body bath was measured using rotating viscometer (Visco-895, ATAGO, Japan) as per the protocol described in SOP No. CL1.2. Viscosity of body bath was measured using Ultra Low Adaptor (ULA) spindle which speeds from 50 to 100 rpm at room temperature.
[096] Viscosity of the body bath formulation changes gradually with increase in rpm value of the spindle. The formulation of the body bath was considered as pseudoplastic behavior as the viscosity decreases with increase in rpm. Pseudoplastic behavior is a desirable attribute in bodybath formulation. All the formulations followed a pseudoplastic rheogram. There was no considerable change in the viscosity of the bodybath formulation from 0 to 30 days with obtained viscosity in the range of 1.6 to 2.8 (Table 7). It was also observed that the complete formulation does not show any significant change in their viscosity from 0 to 30 days at different stress conditions (Table 8, 9, and 10).
[097] Weight measurement
[098] The weight per milliliter of waterless body bath was measured as per the protocol mentioned in SOP No.CL1.3. To measure the specific gravity of the sample, a clean dry pycnometer was weighed, and 5 ml of body bath was added to the same, exact weight of the body bath was calculated after subtraction of reference value.
[099] The weight of the 10 mL body bath in a clean and dry pycnometer was found to be 1.013 gm. However, no significant change was observed from 0 to 30 days (Table 7, 8, and 9). It was found that the changes of weight have a negligible effect on the stability and efficacy of the formulations. Similarly, no change was observed in the weight from 0 to 30 days at different stress conditions (Table 8, 9 and 10).
[100] Centrifugation Test
[101] The centrifugation test of body bath was carried out as per the protocol described in SOP No.CL1.4. The body bath formulation was centrifuged at 3000 rpm for 30 min at 25 °C. After centrifugation, the organoleptic characteristics, pH value, and homogeneity of the body bath formulation were evaluated macroscopically and technically. The centrifugation test did not show any significant change in the organoleptic characteristics, appearance and homogeneity of the body bath formulation (Table 8). It suggests a good stability of the formulation.
Thermal Stress Test
[102] The thermal stress test of body bath was carried out as per the protocol described in SOP No.CL1.5. In this test, the body bath formulations were subjected to a heated thermostatic water bath system at different temperature from 25 °C to 80 °C with a temperature gradient of 10 °C and holding at each temperature for 30 minutes. The organoleptic characteristics and pH value were evaluated after cooling the samples at room temperature. The pH of the body bath formulation changes during thermal stress test (Table 9). However, other parameters are consistent during thermal stress. No change in organoleptic characteristics, odor, color and appearance was observed.
[103] Freeze defrost cycle
[104] The freeze defrost cycle of body bath was carried out as per the protocol described in SOP No.CL1.6. The formulation was placed in the glass tubes and then kept in a humidity chamber at 4±2°C/24h to 45±2°C/24h and 75% relative humidity. The physical and chemical stability parameters of formulation were evaluated after freeze-defrost cycle.
[105] The physical and chemical properties were same during the freeze defrost cycle from 0 to 30 days (Table 10). There were no significant changes that could be observed in the complete formulation after keeping the formulation in a humidity chamber subjected from 45°C± 75% relative humidity.
[106] Table 7: Stability parameters of body bath formulation without any stress conditions from 0 to 30 days at 3 days of interval
S. No. Parameters 0 day 3
day 6
day 9
day 12
day 15
day 18
day 21 day 24
day 27
day 31
day
1 pH 5.3
±0.2 5.3
±0.2 5.4
±0.3 5.5
±0.1 5.7
±0.2 5.6
±0.3 5.6
±0.2 5.5
±0.3 5.8
±0.3 5.6
±0.1 5.5
±0.1
2 Organoleptic characteristics (color, odor, and appearance) Fresh clear liquid and fresh odor No change No significant change
3 Viscosity 2.0
±0.2 2.1
±0.1 2.3
±0.1 2.3
±0.2 2.3
±0.3 1.9
±0.4 2.0
±0.2 2.1
±0.2 2.3
±0.3 2.1
±0.2 1.9
±0.4
4 Specific gravity 1.034 1.035 1.036 1.034 1.032 1.031 1.032 1.034 1.034 1.032 1.032
5 PDI 0.41
±0.01 0.38
±0.02 0.34
±0.01 0.33
±0.03 0.33
±0.01 0.35
±0.04 0.33
±0.01 0.39
±0.04 0.34
±0.02 0.35
±0.02 0.34
±0.01
6 Foam stability and ability Good foaming, wipe out easily No significant change

[107] Table 8: Stability parameters of body bath formulation after centrifugation stress from 0 to 30 days at 3 days of interval.
S. No. Parameters 0 day 3
day 6
day 9
day 12
day 15
day 18
day 21 day 24
day 27
day 31
day
1 pH 5.3
±0.2 5.4
±0.2 5.4
±0.3 5.6
±0.1 5.8
±0.2 5.7
±0.3 5.4
±0.2 5.5
±0.3 5.5
±0.3 5.5
±0.1 5.5
±0.1
2 Organoleptic characteristics (color, odor, and appearance) Fresh clear liquid and fresh odor No change No significant change
3 Viscosity 2.0
±0.2 2.0
±0.1 2.2
±0.1 2.1
±0.2 2.2
±0.3 2.1
±0.4 2.2
±0.2 2.2
±0.2 2.1
±0.3 2.2
±0.2 2.0
±0.4
4 Specific gravity 1.034 1.089 1.078 1.082 1.091 1.083 1.082 1.072 1.073 1.082 1.082
5 PDI 0.41
±0.03 0.39
±0.04 0.38
±0.05 0.38
±0.06 0.37
±0.04 0.38
±0.03 0.36
±0.02 0.38
±0.03 0.37
±0.04 0.37
±0.05 0.38
±0.04
6 Foam stability and ability wipe out easily No significant change

[108] Table 9: Stability parameters of body bath formulation after thermal stress from 0 to 30 days at 3 days of interval.
S. No. Parameters 0 day 3
day 6
day 9
day 12
day 15
day 18
day 21 day 24
day 27
day 31
day
1 pH 5.3
±0.2 5.4
±0.2 5.4
±0.3 5.6
±0.1 5.8
±0.2 5.7
±0.3 5.4
±0.2 5.5
±0.3 5.5
±0.3 5.5
±0.1 5.5
±0.1
2 Organoleptic characteristics (color, odor, and appearance) Fresh clear liquid and fresh odor No change No significant change
3 Viscosity 2.0
±0.2 2.1
±0.1 2.3
±0.1 2.2
±0.2 2.2
±0.3 2.1
±0.4 2.0
±0.2 2.1
±0.2 2.2
±0.3 2.1
±0.2 2.1
±0.4
4 Specific gravity 1.034 1.048 1.044 1.047 1.048 1.049 1.051 1.043 1.044 1.032 1.037
5 PDI 0.41
±0.03 0.40
±0.04 0.42
±0.05 0.40
±0.06 0.41
±0.04 0.41
±0.03 0.42
±0.02 0.43
±0.03 0.44
±0.04 0.42
±0.05 0.44
±0.04
6 Foam stability and ability wipe out easily No significant change , slightly yellowish

[109] Table 10: Stability parameters of body bath formulation after freeze defrost stress from 0 to 30 days at 3 days of interval.
S. No. Parameters 0 day 3
day 6
day 9
day 12
day 15
day 18
day 21 day 24
day 27
day 31
day
1 pH 5.5
±0.1 5.5
±0.2 5.5
±0.1 5.5
±0.2 5.4
±0.2 5.3
±0.2 5.6
±0.1 5.7
±0.2 5.6
±0.1 5.7
±0.2 5.8
±0.2
2

Organoleptic characteristics (color, odor, and appearance) Fresh clear liquid and fresh odor No change

No significant change
3 Viscosity 2.0
±0.2 2.1
±0.1 2.2
±0.3 2.3
±0.4 2.1
±0.5 2.2
±0.4 2.3
±0.3 2.4
±0.4 2.3
±0.4 2.3
±0.4 2.0
±0.3
4 Specific gravity 1.034 1.042 1.043 1.044 1.045 1.044 1.043 1.044 1.043 1.042 1.037
5 PDI 0.41
±0.02 0.42
±0.03 0.41
±0.04 0.41
±0.05 0.43
±0.03 0.42
±0.02 0.41
±0.03 0.41
±0.04 0.42
±0.03 0.43
±0.03 0.42
±0.02
6 Foam stability and ability wipe out easily No significant change , slightly yellowish

Conclusion
[110] It was found that waterless body bath formulation was very stable for one month. Preliminary studies suggest that there was no substantial change in the chemical, physical, and organoleptic characteristics of the formulation upon subjected to various stress conditions from 0 to 30 days.
Dermatological safety Test
[111] The study was designed to test the safety of topical product. The study was designed to test the safety of the waterless body bath composition by 24 hours patch test under complete occlusion on healthy human subjects. The control taken was 3% sodium lauryl sulphate in distilled water. The product under investigation was evaluated through single application closed patch test under occlusion for 24 hours. After patch removal, skin was observed for irritation reactions at 30 mins, 24 hrs, 48 hrs and 7 days post patch removal for immediate as well as delayed reactions.
Investigational
Product Mean Irritation Score- 0 Hr Irritancy assessment Mean Irritation Score- 24 Hrs Irritancy assessment Mean Irritation Score- 48 Hrs Irritancy assessment Mean Irritation Score- 7 days Irritancy assessment
Waterless
Body bath 0.00 Non
Irritant 0.00 Non
Irritant 0.00 Non
Irritant 0.00 Non
Irritant
Positive Control 5.41 Irritant 4.87 Irritant 3.79 Mild Irritant 0.16 Subsiding Mild Irritation
[112] Average mean skin irritation score for each tested formulation is tabulated below:

[113] As per Draize scale for scoring irritation, the waterless body bath composition of the present invention emerged as non-irritant when observed at 0hr, 24 hours, 48 hours and at 7 days later. The waterless body bath compositions were deemed to be dermatologically safe as per their classification into non-irritant category at all time points of evaluation by 24 hrs occlusive patch test methods. Positive control was confirmed as irritant when observed at 0hr, 24 hrs and end of 7th day of removal of the patch.
, C , Claims:WE CLAIM:

1. A waterless body cleaning composition comprising:
a. A primary cationic surfactant from 0.5% to 2% by weight of the total composition (wt/wt);
b. a secondary surfactant from 0.5% to 2% (wt/wt);
c. one or more antimicrobial and/or antibacterial compound or disinfectant from 0.1% to 2% (wt/wt);
d. at least one humectant/moisturising agent/ antifreezing agent from 0.5% to 2% (wt/wt);
e. at least one preservative from 0.01% to 0.1% (wt/wt);
f. at least one modifier/pH controller from 0.1% to 1.0%% (wt/wt);
g. at least one fragrance from 0.001% to 2% by weight of the total composition; and
h. a solvent
2. The composition as claimed in claim 1, wherein the primary cationic surfactant is selected from the group consisting of capryl glucoside, caprylyl glucoside or a combination thereof.
3. The composition as claimed in claim 1, wherein the secondary surfactant is cocamidopropyl betaine..
4. The composition as claimed in claim 1, wherein the preservative is selected from the group comprising of citric acid, benzoic acid, phenoxyethanol or analogue thereof, sorbic acid, or a combination thereof.
5. The composition as claimed in claim 1, wherein an antimicrobial agent/antibacterial/disinfectant is selected from the group comprising of a strong base with cationic properties such as chlorhexidine digluconate, sodium benzoate, dehydroacetic acid or a combination thereof.
6. The composition as claimed in claim 1, wherein the humectant/moisturising agent/ antifreezing agent is selected from the group consisting of propylene glycol, glycerine, plant oils, lactic acid and panthenol or mixtures thereof.
7. The composition as claimed in claim 1, wherein the modifier/pH controller is selected from the group comprising of citric acid, disodium EDTA, sodium hydroxide or a combination thereof.
8. The composition as claimed in claim 1, wherein the fragrance is selected from the group comprising of absolute repair, intense repair, lavender, rose, citrus and natural fragrance or combinations thereof.
9. The composition as claimed in claim 1, wherein the composition shows an anti-microbial efficacy of 99.9% within 30 seconds of use.
10. A waterless formulation comprising composition as claimed in claim 1, wherein the formulation is selected from the group of body-bath, tooth-paste, shampoo, face cleanser and the like.