An improved preservative blend with antimicrobial properties

Abstract

The present invention relates to a multifunctional preservative system that provides effective broad spectrum microbial protection while delivering ancillary benefits such as anti-acne, anti-dandruff, and anti-plaque properties. The present invention offers a novel approach to preservation, addressing the limitations of traditional preservatives such as parabens and formaldehyde donors. The preservative formulation synergistically combines antibacterial properties of organic bases, the antifungal activity of organic acids, and the structural and stabilizing benefits of organic acid salts.

Description

AN IMPROVED PRESERVATIVE BLEND WITH ANTIMICROBIAL PROPERTIESBACKGROUNDTechnical Field of Invention

[0001] The embodiments herein generally relate to the field of personal care and cosmetic product preservation formulations. More specifically, the embodiments herein relate to a multifunctional preservative system that provides effective antimicrobial protection while delivering ancillary benefits such as anti-acne, antidandruff, and anti-plaque properties.Description of Related Art

[0002] The personal care and cosmetic industry are one of the fastest-growing industry in global markets. This dynamic sector continually introduces innovative ideas, new ingredients, and novel claims. With rapid growth comes diversification into multiple product categories, each requiring robust preservation systems to ensure product safety, efficacy, and shelf stability.

[0003] Traditional preservatives, such as parabens and formaldehyde donors, are increasingly being phased out due to their potential adverse reactions and growing consumer concerns. Consequently, there is a heightened demand for preservative systems that are stable, effective, and functions efficiently at low concentrations.

[0004] Hence there is a need to develop a preservative blend formulation that is efficient, stable, has anti-microbial properties and which is effective in low concentrations. There is also a need to develop a stable blend which can be combined with various compounds successfully to bring out stable anti-microbial formulations.

[0005] The value additions and above-mentioned shortcomings, disadvantages and problems are addressed herein, as detailed below.SUMMARY OF THE INVENTION

[0006] The primary objective of the embodiments herein is to provide an improved preservative blend formulation having anti-microbial properties.

[0007] Yet another objective of the embodiments herein in to provide a preservative blend that is stable, efficient and effective in lower concentrations.

[0008] Yet another objective of the embodiments herein is to provide a preservative blend having synergistically combined antibacterial properties of organic bases, the antifungal activity of unsaturated organic acids, and the structural and stabilizing benefits of saturated & aromatic organic acid salts.

[0009] Yet another objective of the embodiments herein in to provide a preservative blend providing additional benefits such as anti-acne, anti-dandruff, anti-plaque properties.

[0010] Yet another objective of the embodiments herein is to provide a preservative blend that is compatible with personal care and cosmetic formulations across various categories, including skin care, skin cleansing, hair care, and oral care.

[0011] Yet another objective of the embodiments herein is to provide a preservative blend having multifunctional properties, thereby reducing the need for additional active ingredients, simplifying formulations, and lowering costs.

[0012] Yet another objective of the embodiments herein is to provide a preservative blend which works well at low concentration usage also thereby ensuring minimal interference with the sensory properties of the final product.

[0013] Yet another objective of the embodiments herein is to provide a preservative blend which can be prepared into various forms such as hand wash, antiacne face wash, antidandruff shampoo, mouth wash, wet wipe solution, face cream, and face wash.

[0014] The various embodiments herein provide a preservative blend formulation having anti-microbial properties. The preservative blend comprises one or more therapeutically active compound, one or more organic acid, and an organic acid salts.

[0015] According to an embodiment herein, a preservative blend formulation having anti-microbial properties is provided. The preservative blend formulationcomprises a therapeutically active compound, an undecylenic acid and one or more organic acid.

[0016] According to an embodiment herein, the therapeutically active compound is Chlorhexidine.

[0017] According to an embodiment herein, the preservative blend composition comprises undec- 10-enoic acid.

[0018] According to an embodiment herein, the one or more organic acid / aliphatic or aromatic acid comprises benzoic acid, sorbic acid, salicylic acid, dehydroacetic acid, and levulinic acid.

[0019] According to an embodiment herein, the therapeutically active compound is present in a quantity of 54%-60% by weight.

[0020] According to an embodiment herein, the undec- 10-enoic acid is present in a quantity of 40%-46% by weight.

[0021] According to an embodiment herein, the organic acid / aliphatic or aromatic acid is present in a quantity of 2%-3% by weight.

[0022] According to an embodiment herein, the preservative blend works efficiently at a low concentration of up to 0.1% to 0.5%.

[0023] According to an embodiment herein, the preservative blend can be used for the preservation in face cream, a Face wash, a hair mask, a wet wipes, and a mouth wash formulation.

[0024] According to another embodiment herein, a method of synthesizing a preservative blend formulation having anti-microbial properties is provided. The method comprises adding a solvent into a reactor (101), wherein the solvent is an alcohol. Further, adding an undecylenic acid and an organic acid into the reactor while slowly purging nitrogen gas at room temperature to obtain a slurry (102). The slurry is stirred (103). The chlorhexidine is gradually added to the reactor to adjust the pH between 6.5 to 7.5 over a period to get a clear solution (104). The solution is cooled down to room temperature till crystals are formed (105). The crystals are separated by filtration (106). The organic acid is selected from the group consisting of benzoic acid, sorbic acid, salicylic acid, hydroxamic acid, dehydroacetic acid, and levulinic acid. The undecylenic acid is added in an amount of 40%-46% byweight. The organic acid is added in an amount of 2%-3% by weight. The chlorhexidine is added in a quantity of 54%-60% by weight.

[0025] According to an embodiment herein, the one or more organic acid comprises undecylenic acid, hydroxamic acid, benzoic acid, sorbic acid, salicylic acid, dehydroacetic acid, and levulinic acid.

[0026] The blend comprises of a broad-spectrum preservative moiety. The preservation blend comprises anti-bacterial as well as anti-fungal activity.

[0027] According to an embodiment herein, the preservative blend can be used into various formulations such as hand wash, antiacne face wash, antidandruff shampoo, mouth wash, wet wipe solution, face cream, and face wash.

[0028] These and other aspects of the embodiments herein will be better appreciated and understood when considered in conjunction with the following description and the accompanying drawings. It should be understood, however, that the following descriptions, while indicating preferred embodiments and numerous specific details thereof, are given by way of illustration and not of limitation. Many changes and modifications may be made within the scope of the embodiments herein without departing from the spirit thereof, and the embodiments herein include all such modifications.BRIEF DESCRIPTION OF DRAWINGS

[0029] The other objects, features and advantages will occur to those skilled in the art from the following description of the preferred embodiment and the accompanying drawings in which:

[0030] FIG. 1 is a flow chart showing the various steps involved in the method of synthesizing a preservative blend formulation having anti-microbial properties, according to an embodiment herein.DETAILED DESCRIPTION OF EMBODIMENTS

[0031] In the following detailed description, a reference is made to the accompanying drawings that form a part hereof, and in which the specificembodiments that may be practiced is shown by way of illustration. The embodiments are described in sufficient detail to enable those skilled in the art to practice the embodiments and it is to be understood that the logical, mechanical, electronic and other changes may be made without departing from the scope of the embodiments. The following detailed description is therefore not to be taken in a limiting sense.

[0032] The various embodiments herein relate to an innovative preservative blends designed to enhance the stability, safety, and efficacy of personal care and cosmetic formulations. The preservative systems can synergistically combine the antibacterial properties of organic bases, the antifungal activity of organic acids, and the structural and stabilizing benefits of organic acid salts.

[0033] According to the embodiments herein, the preservative blend formulation comprises one or more therapeutically active compound, one or more organic acid, and a salt of sodium.

[0034] According to an embodiment herein, the one or more therapeutically active compound comprises one or more anti-microbial agents.

[0035] According to an embodiment herein, the one or more organic acid comprises Undecylenic Acid, Hydroxamic Acid, Benzoic Acid, Sorbic Acid, Salicylic Acid, , Dehydroacetic Acid, and Levulinic Acid.

[0036] FIG. 1 is a flow chart showing the various steps involved in the method of synthesizing a preservative blend formulation having anti-microbial properties, according to an embodiment herein. With respect to FIG. 1, the method of synthesizing a preservative blend formulation having anti-microbial properties comprises adding a solvent into a reactor (101), wherein the solvent is alcohol. Further, adding an undecylenic acid and an organic acid into the reactor while slowly purging nitrogen gas at room temperature to obtain a slurry (102). The slurry is stirred for one hour (103). The chlorhexidine is gradually added to the reactor to adjust the pH between 6.5 to 7.5 over a period to get a clear solution (104). The solution is cooled down to room temperature till crystals are formed (105). The crystals are separated by filtration (106). The organic acid is selected from the group consisting of benzoic acid, sorbic acid, salicylic acid, hydroxamic acid,dehydroacetic acid, and levulinic acid. The undecylenic acid is added in an amount of 40%-46% by weight. The organic acid is added in an amount of 2%-3% by weight. The chlorhexidine is added in a quantity of 54%-60% by weight.

[0037] These components are carefully blended to deliver broad-spectrum antimicrobial efficacy at minimal concentrations.

[0038] According to the embodiment herein, a novel method of synthesizing an antibacterial and antifungal compositions is provided. The composition comprises Chlorohexidine, Undecylenic acid and other acids e.g. Benzoic acid

[0039] According to an embodiment herein, an alcoholic solution of Chlorhexidine, Undecylenic acid, and Benzoic acid is prepared. The organic solvent is distilled off, and the resulting solid formed as a precipitate is filtered and dried to obtain a final product.

[0040] According to another embodiment herein, an alcoholic solution of Chlorhexidine, Undecylenic acid, and Sorbic acid is prepared. The organic solvent is distilled off, and the resulting solid formed as a precipitate is filtered and dried to obtain a final product.

[0041] According to another embodiment herein, an alcoholic solution of Chlorhexidine, Undecylenic acid, and Salicylic acid is prepared. The organic solvent is distilled off, and the resulting solid formed as a precipitate is filtered and dried to obtain a final product.

[0042] According to another embodiment herein, an alcoholic solution of Chlorhexidine, Undecylenic acid, and Dehydroacetic acid is prepared. The organic solvent is distilled off, and the resulting solid formed as a precipitate is filtered and dried to obtain a final product.

[0043] According to another embodiment herein, an alcoholic solution of Chlorhexidine, Undecylenic acid, and Levulinic acid is prepared. The organic solvent is distilled off, and the resulting solid formed as a precipitate is filtered and dried to obtain a final product.

[0044] According to an embodiment herein, a blend of chlorhexidine base with and organic acid (which is converted into its salt insitu) and a third ingredient which isalso an organic acid. The second acid plays a role of both antifungal and preservative active.

[0045] According to an embodiment herein, the chlorhexidine base and the organic acid work in synergism with each other. The blend of chlorhexidine base and the organic acid when mixed is converted to sodium salt insitu. The acid is undecylenic acid. The other acid, is acids / or acid sodium salt such as hydroxamic acid, benzoic acid, sorbic acid, salicylic acid, dehydroacetic acid, and levulinic acid).

[0046] According to the embodiments herein, and as a part of this innovative effort, the preservative blends utilize Chlorhexidine Base, a highly effective antimicrobial agent, as the core organic amine. This is combined with a variety of organic acids and their salts to achieve comprehensive antimicrobial protection. The selected organic acids include Undecylenic Acid, Hydroxamic Acid, Benzoic Acid, Sorbic Acid, Salicylic Acid, Dehydroacetic Acid, and Levulinic Acid. These components are carefully blended to deliver broad-spectrum antimicrobial efficacy at minimal concentrations.

[0047] The present invention provides an innovative and highly effective preservative blend designed for use in personal care and cosmetic formulations. It offers broad-spectrum antimicrobial activity against bacteria and fungi, ensuring product stability and safety. Comprising Undecylenic Acid, Chlorhexidine Base, and organic acids, the composition / formulations of the present invention combine preservation efficacy with additional functional benefits, including anti-acne, antidandruff, and anti-plaque properties. This multifunctional preservative works efficiently at a low concentration of up to 0.3%, making it a cost-effective and versatile solution for various product categories, including skin care, skin cleansing, hair care, and oral care.

[0048] According to an embodiment herein, the preservative blend is prepared into various forms such as hand wash, antiacne face wash, antidandruff shampoo, mouth wash, wet wipe solution, face cream, and face wash.

[0049] Table 1 shows a stable and synergistic composition blend of preferred antimicrobial agent. The product is named as “Tricloshield”, wherein the term“Tricloshield” is interchangeably used with the “stable composition” and “composition of the present invention” as per the present invention.Table 1 showing the stable composition

[0050] Undecylenic acid is a natural antimicrobial agent derived from castor oil, known for its effectiveness against fungi and bacteria. Undecylenic acid is an active ingredient in medications for skin infections, and to relieve itching, burning, and irritation associated with skin problems. Undecylenic acid is an active ingredient in medications for skin infections, and to relieve itching, burning, and irritation associated with skin problems.

[0051] Chlorhexidine is a potent antimicrobial agent with additional benefits for oral care and skin applications. Chlorhexidine is an antiseptic and disinfectant that is used to treat skin and mouth infections.

[0052] Undecylenic acid is widely used preservative recognized for its antimicrobial properties, particularly against fungi.

[0053] The components of Tricloshield / stable composition of the present invention work synergistically to inhibit microbial growth, ensuring product safety. Undecylenic Acid disrupts the cell membranes of microorganisms, Chlorhexidine Base provides bactericidal and bacteriostatic effects.

[0054] The formulations prepared according the present invention are highly effective in providing broad- Spectrum antimicrobial activity. These blendseffectively inhibit the growth of bacteria, fungi-mold and yeasts, providing comprehensive protection against microbial contamination.

[0055] The formulations prepared according the present invention has enhanced stability. The inclusion of organic acid salts as fillers improves the stability and compatibility of the blends within a wide range of formulations and pH levels.

[0056] The formulations prepared according the present invention are highly effective at lower dosages and hence reduce the usage levels. The synergistic combination of organic bases, acids, and their salts allows for effective preservation at low concentrations, reducing interference with the sensory and functional properties of the final product.

[0057] The formulations prepared according the present invention have multifunctional benefits. In addition to antimicrobial protection, certain organic acids (e.g., Salicylic Acid) offer additional benefits such as exfoliation, antiinflammatory effects, and enhanced skin care performance.

[0058] The formulations prepared according the present invention are customizable formulations. The preservative blends can be tailored by varying the combinations of organic acids and their salts to suit specific formulation requirements and regulatory standards.

[0059] The formulations prepared according the present invention are consumer and environment friendly. These preservative systems exclude controversial ingredients like parabens and formaldehyde donors, catering to the growing demand for safer and more sustainable products.

[0060] The formulations prepared according the present invention are versatile across applications such as the preservative blends are suitable for a wide range of personal care and cosmetic products, including skin care, hair care, oral care, home care and cleansing formulations.

[0061] According to an embodiment of the present invention, the stable composition / Tricloshield is versatile and can be incorporated into various personal care and cosmetic formulations:

[0062] Skin Care: Suitable for acne creams, foundations, serums, lipsticks, powders, and sunscreen formulations.

[0063] Skin Cleansing: Effective in body washes, soaps, and hand washes.

[0064] Hair Care: Ideal for shampoos, conditioners, hair serums, and hair masks.

[0065] Oral Care: Provides preservation and functional benefits in toothpaste, mouthwash, and toothpaste tablets.

[0066] Home Care: Provide antimicrobial efficacy in liquid dishwash, floor cleaner, bathroom cleaner.

[0067] Hence, the novel preservative blends, as per the present invention, show stability and enhance antimicrobial efficacy. Tricloshield represents a significant advancement in preservative technology, offering an effective, multifunctional, and consumer-friendly solution for the preservation needs of the rapidly evolving personal care and cosmetic industry.

[0068] The following specification will now be explained by means of examples. It is to be noted that the following examples are not to be used in any limiting sense.EXAMPLE 1

[0069] Synthesis of antibacterial and antifungal composition of Chlorhexidine, Undecylenic acid and Benzoic acid: Charge 4000 mL of alcohol into a glass reactor. Under slow purging of nitrogen at room temperature, add Undecylenic acid (505.2 g, 1.0 mol) and Benzoic acid to the reactor. Stir the resulting slurry and adjust the pH 6.5 to 7.5 by the gradual addition of Chlorhexidine base. Continue stirring the reaction mass till it is clear. Cool the reaction mixture to room temperature to induce crystallization. Isolate the final product by filtration and dry it to obtain the desired compound.

[0070] The analysis of the above antibacterial and antifungal composition is shown in Table A:Table A: showing the analysis of composition comprising Chlorhexidine, Undecylenic acid and Benzoic acidEXAMPLE 2

[0071] Synthesis of antibacterial and antifungal composition of Chlorhexidine, Undecylenic acid and Sorbic acid: Charge 4000 mL of alcohol into a glass reactor. Under slow purging of nitrogen at room temperature, add Undecylenic acid (505.2 g, 1.0 mol) and Sorbic acid to the reactor. Stir the resulting slurry for 1 hour. Adjust the pH 6.5 to 7.5 by the gradual addition of Chlorhexidine base over a period of 1 hour to get clear solution. Continue stirring the reaction mass for an additional 2 hours. Cool the reaction mixture to room temperature to induce crystallization. Isolate the final product by filtration and dry it to obtain the desired compound.

[0072] The analysis of the above antibacterial and antifungal composition is shown in Table B.Table B showing the analysis of the composition comprising Chlorhexidine,Undecylenic acid and Sorbic acidEXAMPLE 3

[0073] Synthesis of antibacterial and antifungal composition of Chlorhexidine, Undecylenic acid and Salicylic acid: Charge 4000 mL of alcohol into a glass reactor. Under slow purging of nitrogen at room temperature, add Undecylenic acid (505.2 g, 1.0 mol) and Salicylic acid to the reactor. Stir the resulting slurry at SO-55 °C for 1 hour. Adjust the pH 6.5 to 7.5 by the gradual addition of Chlorhexidine base over a period of 1 hour to get clear solution. Continue stirring the reaction mass at 50-55 °C for an additional 2 hours. Cool the reaction mixture to room temperature to induce crystallization. Isolate the final product by filtration and dry it to obtain the desired compound.

[0074] The analysis of the above antibacterial and antifungal composition is shown in Table C.Table C showing the analysis of the composition comprising Chlorhexidine,Undecylenic acid and Salicylic acidEXAMPLE 4

[0075] Synthesis of antibacterial and antifungal composition of Chlorhexidine, Undecylenic acid and Dehydoacetic acid: Charge 4000 mL of alcohol into a glassreactor. Under slow purging of nitrogen at room temperature, add Undecylenic acid (505.2 g, 1.0 mol) and Dehydroacetic acid to the reactor. Stir the resulting slurry at 50-55 °C for 1 hour. Adjust the pH 6.5 to 7.5 by the gradual addition of Chlorhexidine base over a period of 1 hour to get clear solution. Continue stirring the reaction mass at 50-55 °C for an additional 2 hours. Cool the reaction mixture to room temperature to induce crystallization. Isolate the final product by filtration and dry it to obtain the desired compound.

[0076] The analysis of the above antibacterial and antifungal composition is shown in Table D.Table D showing the analysis of the composition comprising Chlorhexidine,Undecylenic acid and Dehydoacetic acidEXAMPLE 5

[0077] Synthesis of antibacterial and antifungal composition of Chlorhexidine, Undecylenic acid and Levulinic acid: Charge 4000 mL of alcohol into a glass reactor. Under slow purging of nitrogen at room temperature, add Undecylenic acid (505.2 g, 1.0 mol) and Levulinic acid to the reactor. Stir the resulting slurry at SO-55 °C for 1 hour. Adjust the pH 6.5 to 7.5 by the gradual addition of Chlorhexidine base over a period of 1 hour to get clear solution. Continue stirring the reaction mass at 50-55 °C for an additional 2 hours. Cool the reaction mixture to roomtemperature to induce crystallization. Isolate the final product by filtration and dry it to obtain the desired compound.

[0078] The analysis of the above antibacterial and antifungal composition is shown in Table E.Table E showing the analysis of the composition comprising Chlorhexidine,Undecylenic acid and Levulinic acidEXPERIMENTAL DETAILS

[0079] According to the embodiments of the present invention, the composition of the present invention is made into various forms, wherein the forms are face cream, Face wash, hair mask, wet wipes, and mouth wash.

[0080] Below examples show the efficacy tests for the various dosage forms.Preservative Efficacy Test (PET) for FACE CREAM

[0081] Name of Test : USP <51> Antimicrobial Effectiveness Testing

[0082] Scope of Test: This method provides test to demonstrate the Effectiveness of Antimicrobial protection for Topically Used Formulation. The formulation is a face cream.

[0083] Principle: The evaluation of the preservation of a cosmetic formulation is based on inoculation of the formulation with calibrated inoculum prepared fromrelevant strains of micro-organisms. The number of surviving micro-organisms is measured at defined intervals during a period of 28 days. For each time and each strain, the log reduction value is calculated.

[0084] Test Organisms: Staphylococcus aureus ATCC 6538, Escherichia coli ATCC 8739, Pseudomonas aeruginosa ATCC 9027, Aspergillus brasiliensis ATCC 16404, Candida albicans ATCC 10231.

[0085] Table 2.1 below shows the product preparation and experimental conditions for the test.Table 2.1 product preparation and experimental condition for face cream

[0086] Table 2.2 shows the details of the Product Sterility Test for face cream.Table 2.2 Product sterility Test< <

[0087] Table 2.3 shows the details of the Experimental Condition Validation, wherein Control Nv= Inoculum control, Control Nvn= Control, and Control Nvf= Test.Table 2.3 Experimental Condition Validation for face creamWhere -Vc = Count per ml, x = Average of Vcl and Vc2

[0088] Verification of Method:

[0089] Microbial suspension (N) = Bacterial culture standardized to 1^107 / 108 CFU / ml; Fungi 1x106 / 107 CFU / ml , while Nv shall be about 100. The efficacy of the neutralizer is demonstrated if Nvf > 0.5Nvn and if Nvn is close to Nv. If Nvn is not close to Nv, the neutralizer is considered toxic for micro-organisms.

[0090] Test Procedure: 20 g or 20 ml of the test formulation was transferred to a sterile container. Then, 0.2 ml of Microbial suspension was added to the test formulation individually to obtain between IxlO5CFU / ml to IxlO6CFU / ml or g for bacteria and between IxlO4CFU / ml to 1 x 105CFU / ml or g for yeast and Molds.Containers holding the inoculated formulation were stored at 22.5 ±2.5 °C. At each specified sampling intervals, 1 g or 1 ml of the inoculated formulation was added to 9 ml of neutralizer. It was mixed until homogeneous. Starting from the 1 / 10 dilution in the neutralizer, successive tenfold dilutions were carried out usingdiluent to perform the enumeration of surviving micro-organisms. Microbial enumeration was carried out using TSA for bacteria, SDA for yeast or PDA for molds. This was performed in duplicate by standard pour plate method. Plates were Incubated at 35 ± 2°C / 24 hrs. for bacteria, at 25 ± 2 °C / 2-3 days for yeast and 5 days for Molds.

[0091] Table 2.4 shows the details of the Test Suspension (N and No) used.Table 2.4: Test Suspension (N and No)

[0092] Table 2.5 show the results obtained. According to table 2.5, the Nx = No. of surviving micro-organisms at each sampling time, NO = No. of micro-organisms inoculated at time 0, and R = Reduction in microbial counts Microbial Reduction = Rx = IgNO - IgNx.Table 2.5: Results< < > < < > < < > < < >< < > < < > < < > < < >< < > < < > < < > < < >< < > < < > < < > < < >< < > < < > < < > < < >

[0093] Criteria for Effectiveness of Preservative:

[0094] 1. > 2 log reduction or No increase in Bacterial count at 14 days and beyond

[0095] 2. No increase in Fungal count at 14 days and 28 days

[0096] As per table 2.5, it was found that the Test product Face Cream complies the requirements of Antimicrobial Effectiveness when tested as per USP <51>.Preservative Efficacy Test (PET) for FACE WASH

[0097] Name of Test : USP <51> Antimicrobial Effectiveness Testing

[0098] Scope of Test: This method provides test to demonstrate the Effectiveness of Antimicrobial protection for Topically Used Formulation. The formulation is Face wash.

[0099] Principle: The evaluation of the preservation of a cosmetic formulation is based on inoculation of the formulation with calibrated inocula prepared from relevant strains of micro-organisms. The number of surviving micro-organisms is measured at defined intervals during a period of 28 days. For each time and each strain, the log reduction value is calculated.

[0100] Test Organisms: Staphylococcus aureus ATCC 6538, Escherichia coli ATCC 8739, Pseudomonas aeruginosa ATCC 9027, Aspergillus brasiliensis ATCC 16404, Candida albicans ATCC 10231.

[0101] Table 3.1 below shows the product preparation and experimental conditions for the test.Table 3.1 product preparation and experimental condition for face wash

[0102] Table 3.2 shows the details of the Product Sterility Test for face wash.Table 3.2 Product sterility Test< <

[0103] Table 3.3 shows the details of the Experimental Condition Validation, wherein Control Nv = Inoculum control, Control Nvn = Control, and Control Nvf = Test.Table 3.3 Experimental Condition Validation for face washWhere : Vc = Count per ml, x = Average of Vcl and Vc2

[0104] Verification of Method:

[0105] Microbial suspension (N) = Bacterial culture standardized to P IO7 / 108CFU / ml; Fungi l*106 / 107CFU / ml, Nv shall be about 100. The efficacy of the neutralizer is demonstrated if Nvf > 0.5Nvn and if Nvn is close to Nv. If Nvn is not close to Nv, the neutralizer is considered toxic for micro-organisms.

[0106] Test Procedure: 20 g or 20 ml of the test formulation was transferred to a sterile container. Then, 0.2 ml of Microbial suspension was added to the test formulation individually to obtain between P IO5CFU / ml to P IO6CFU / ml or g for bacteria and between PIO4CFU / ml to P IO5CFU / ml or g for yeast and Molds. The containers holding the inoculated formulation were stored at 22.5 ± 2.5 °C. At each specified sampling intervals, 1 g or 1 ml of the inoculated formulation was added to 9 ml of neutralizer. It was mixed until homogeneous.Starting from the 1 / 10 dilution in the neutralizer, successive tenfold dilutions were carried out using diluent to perform the enumeration of surviving micro-organisms.Microbial enumeration was carried out using TSA for bacteria, SDA for yeast or PDA for molds. This was performed in duplicate by standard pour plate method.Plates were Incubated at 35 ± 2°C / 24 hrs. for bacteria, at 25 ± 2 °C / 2-3 days for yeast and 5 days for Molds.

[0107] Table 3.4 shows the details of the Test Suspension (N and No) used.Table 3.4: Test Suspension (N and No)

[0108] Table 3.5 show the results obtained. According to Table 3.5, the Nx = No. of surviving micro-organisms at each sampling time, NO = No. of micro-organisms inoculated at time 0, and R = Reduction in microbial counts Microbial Reduction = Rx = IgNO - IgNx.Table 3.5: Results< < > < < > < < > < < >< < > < < > < < > < < >< < > < < > < < > < < >< < > < < > < < > < < >< < > < < > < < > < < >

[0109] Criteria for Effectiveness of Preservative:

[0110] 1. > 2 log reduction or No increase in Bacterial count at 14 days and beyond

[0111] 2 No increase in Fungal count at 14 days and 28 days

[0112] As per Table 3.5, it was found that the test product Face Wash complies the requirements of Antimicrobial Effectiveness when tested as per USP <51>Preservative Efficacy Test (PET) for Hair Mask

[0113] Name of Test : USP <51> Antimicrobial Effectiveness Testing

[0114] Scope of Test: This method provides test to demonstrate the Effectiveness of Antimicrobial protection for Topically Used Formulation.

[0115] Principle: The evaluation of the preservation of a cosmetic formulation is based on inoculation of the formulation with calibrated inocula prepared from relevant strains of micro-organisms. The number of surviving micro-organisms is measured at defined intervals during a period of 28 days. For each time and each strain, the log reduction value is calculated.

[0116] Test Organisms : Staphylococcus aureus ATCC 6538, Escherichia coli ATCC 8739, Pseudomonas aeruginosa ATCC 9027, Aspergillus brasiliensis ATCC 16404, Candida albicans ATCC 10231

[0117] Table 4.1 below shows the product preparation and experimental conditions for the test.Table 4.1 product preparation and experimental condition for face cream

[0118] Table 4.2 shows the details of the Product Sterility Test for face cream.Table 4.2 Product sterility Test< <

[0119] Table 4.3 shows the details of the Experimental Condition Validation, wherein Control Nv= Inoculum control, Control Nvn= Control, and Control Nvf= Test.Table 4.3 Experimental Condition Validation for Hair MaskWhere - Vc = Count per ml, x = Average of Vcl and Vc2

[0120] Verification of Method:

[0121] Microbial suspension (N) = Bacterial culture standardized to I MO7 / 108CFU / ml; Fungi 1x106 / 107 CFU / ml, while Nv shall be about 100. The efficacy of the neutralizer is demonstrated if Nvf > 0.5Nvn and if Nvn is close to Nv. If Nvn is not close to Nv, the neutralizer is considered toxic for microorganisms.

[0122] Test Procedure: 20 g or 20 ml of the test formulation was transferred to a sterile container. Then, 0.2 ml of Microbial suspension was added to the test formulation individually to obtain between IxlO5CFU / ml to IxlO6CFU / ml or g for bacteria and between U I04CFU / ml to IxlO5CFU / ml or g for yeast and Molds. Containers holding the inoculated formulation were stored at 22.5 ± 2.5 °C. At each specified sampling intervals, 1 g or 1 ml of the inoculated formulation was added to 9 ml of neutralizer. It was mixed until homogeneous.Starting from the 1 / 10 dilution in the neutralizer, successive tenfold dilutions were carried out using diluent to perform the enumeration of surviving micro-organisms.Microbial enumeration was carried out using TSA for bacteria, SDA for yeast or PDA for molds. This was performed in duplicate by standard pour plate method.Plates were Incubated at 35 ± 2°C / 24 hrs. for bacteria, at 25 ± 2 °C / 2-3 days for yeast and 5 days for Molds.

[0123] Table 4.4 shows the details of the Test Suspension (N and No) used.Table 4.4: Test Suspension (N and No)

[0124] Table 4.5 show the results obtained. According to table 4.5, the Nx= No. of surviving micro-organisms at each sampling time, NO = No. of microorganisms inoculated at time 0, R = Reduction in microbial counts, Microbial Reduction = Rx = IgNO - IgNxTable 4.5: Results< < > < < > < < > < < >< < > < < > < < > < < >< < > < < > < < > < < >< < > < < > < < > < < > < < > < < > < < > < < >

[0125] Criteria for Effectiveness of Preservative:

[0126] 1. > 2 log reduction or No increase in Bacterial count at 14 days and beyond

[0127] 2. No increase in Fungal count at 14 days and 28 days

[0128] As per table 4.5, it was found that the test product Hair Mask complies the requirements of Antimicrobial Effectiveness when tested as per USP <51>Preservative Efficacy Test (PET) for Wet Wipes

[0129] Name of Test : USP <51> Antimicrobial Effectiveness Testing

[0130] Scope of Test: This method provides test to demonstrate the Effectiveness of Antimicrobial protection for Topically Used Formulation. The formulation is a wet wipes.

[0131] Principle: The evaluation of the preservation of a cosmetic formulation is based on inoculation of the formulation with calibrated inocula prepared from relevant strains of micro-organisms. The number of surviving microorganisms is measured at defined intervals during a period of 28 days. For each time and each strain, the log reduction value is calculated.

[0132] Test Organisms: Staphylococcus aureus ATCC 6538, Escherichia coli ATCC 8739, Pseudomonas aeruginosa ATCC 9027, Aspergillus brasiliensis ATCC 16404, Candida albicans ATCC 10231.

[0133] Table 5.1 below shows the product preparation and experimental conditions for the test.Table 5.1 product preparation and experimental condition for wet wipes

[0134] Table 5.2 shows the details of the Product Sterility Test for wet wipes.Table 5.2 Product sterility Test< <

[0135] Table 5.3 shows the details of the Experimental Condition Validation, wherein Control Nv= Inoculum control, Control Nvn = Control, and Control Nvf = Test.Table 5.3 Experimental Condition Validation for wet wipes Validation and controlsWhere - Vc = Count per ml, x = Average of Vcl and Vc2

[0136] Verification of Method:

[0137] Microbial suspension (N) = Bacterial culture standardized to P IO7 / 108CFU / ml; Fungi l*106 / 107CFU / ml, while Nv shall be about 100. The efficacy of the neutralizer is demonstrated if Nvf > 0.5Nvn and if Nvn is close to Nv. If Nvn is not close to Nv, the neutralizer is considered toxic for micro-organisms.

[0138] Test Procedure: 20 g or 20 ml of the test formulation was transferred to a sterile container. Then, 0.2 ml of Microbial suspension was added to the test formulation individually to obtain between P IO5CFU / ml to P IO6CFU / ml or g for bacteria and between PIO4CFU / ml to P IO5CFU / ml or g for yeast and Molds. Containers holding the inoculated formulation were stored at 22.5 ± 2.5 °C. At each specified sampling intervals, 1 g or 1 ml of the inoculated formulation was added to 9 ml of neutralizer. It was mixed until homogeneous.Starting from the 1 / 10 dilution in the neutralizer, successive tenfold dilutions were carried out using diluent to perform the enumeration of surviving micro-organisms.Microbial enumeration was carried out using TSA for bacteria, SDA for yeast or PDA for molds. This was performed in duplicate by standard pour plate method.Plates were Incubated at 35 ± 2°C / 24 hrs. for bacteria, at 25 ± 2 °C / 2-3 days for yeast and 5 days for Molds.

[0139] Table 5.4 shows the details of the Test Suspension (N and No) used.Table 5.4: Test Suspension (N and No)= No. of surviving micro-organisms at each sampling time, No = No. of microorganisms inoculated at time 0, and R = Reduction in microbial counts Microbial Reduction = Rx = IgNO - IgNxTable: 5.5: Results:< < > < < > < < > < < >< < > < < > < < > < < >< < > < < > < < > < < >< < > < < > < < > < < >< < > < < > < < > < < >

[0141] Criteria for Effectiveness of Preservative:

[0142] 1. > 2 log reduction or No increase in Bacterial count at 14 days and beyond

[0143] 2 No increase in Fungal count at 14 days and 28 days

[0144] As per table 5.5, it was found that the test product Wet Wipes complies the requirements of Antimicrobial Effectiveness when tested as per USP <51>.Preservative Efficacy Test (PET) for Mouthwash

[0145] Name of Test : USP <51> Antimicrobial Effectiveness Testing

[0146] Scope of Test: This method provides test to demonstrate the Effectiveness of Antimicrobial protection for Topically Used Formulation.

[0147] Principle: The evaluation of the preservation of a cosmetic formulation is based on inoculation of the formulation with calibrated inocula prepared from relevant strains of micro-organisms. The number of surviving microorganisms is measured at defined intervals during a period of 28 days. For each time and each strain, the log reduction value is calculated.

[0148] Test Organisms: Staphylococcus aureus ATCC 6538, Escherichia coli ATCC 8739, Pseudomonas aeruginosa ATCC 9027, Aspergillus brasiliensis ATCC 16404, Streptococcus mutans ATCC 25175, Candida albicans ATCC 10231

[0149] Table 6.1 below shows the product preparation and experimental conditions for the test.Table 6.1 product preparation and experimental condition for Mouthwash

[0150] Table 6.2 shows the details of the Product Sterility Test for face cream.Table 6.2 Product sterility Test< <

[0151] Table 6.3 shows the details of the Experimental Condition Validation, wherein Control Nv = Inoculum control, Control Nvn = Control, and Control Nvf = TestTable 6.3 Experimental Condition Validation for MouthwashWhere - Vc = Count per ml, x = Average of Vcl and Vc2

[0152] Verification of Method:

[0153] Microbial suspension (N) = Bacterial culture standardized to 1^107 / 108 CFU / ml; Fungi 1x106 / 107 CFU / ml, while Nv shall be about 100. The efficacy of the neutralizer is demonstrated if Nvf > 0.5Nvn and if Nvn is close to Nv. If Nvn is not close to Nv, the neutralizer is considered toxic for microorganisms.

[0154] Test Procedure: 20 g or 20 ml of the test formulation was transferred to a sterile container. Then, 0.2 ml of Microbial suspension was added to the test formulation individually to obtain between IxlO5CFU / ml to IxlO6CFU / ml or g for bacteria and between IxlO4CFU / ml to IxlO5CFU / ml or g for yeast and Molds. Containers holding the inoculated formulation were stored at 22.5 ± 2.5 °C. At each specified sampling intervals, 1 g or 1 ml of the inoculated formulation was added to 9 ml of neutralizer. It was mixed until homogeneous.Starting from the 1 / 10 dilution in the neutralizer, successive tenfold dilutions were carried out using diluent to perform the enumeration of surviving micro-organisms.Microbial enumeration was carried out using TSA for bacteria, SDA for yeast or PDA for molds. This was performed in duplicate by standard pour plate method.Plates were Incubated at 35 ± 2°C / 24 hrs. for bacteria, at 25 ± 2 °C / 2-3 days for yeast and 5 days for Molds.

[0155] Table 6.4 shows the details of the Test Suspension (N and No) used.Table 6.4: Test Suspension (N and No)

[0156] Table 6.5 show the results obtained. According to table 2.5, the Nx= No. of surviving micro-organisms at each sampling time, No = No. of microorganisms inoculated at time 0, and R = Reduction in microbial counts Microbial Reduction = Rx = IgNO - IgNxTable 6.5 : Results< < > < < > < < > < < >< < > < < > < < > < < >< < > < < > < < > < < >< < > < < > < < > < < >< < > < < > < < > < < >< < > < < > < < > < < >

[0157] Criteria for Effectiveness of Preservative:

[0158] 1. > 2 log reduction or No increase in Bacterial count at 14 days and beyond

[0159] 2. No increase in Fungal count at 14 days and 28 days

[0160] As per table 6.5, it was found that the test product Mouthwash complies the requirements of Antimicrobial Effectiveness when tested as per USP<51>.Time-Kill / Kill Test: ASTME2315 (2023) OF THE COMPOSITION

[0161] Objective: To quantitatively assess how a test material (e.g. disinfectant, antimicrobial agent) reduces a microbial population over defined time intervals (i.e. its “kill-rate”).

[0162] Scope: Covers in vitro measurement of reduction in aerobic microorganisms under user-specified conditions (organism, exposure time, temperature, etc.).

[0163] Basic Principle / Workflow:

[0164] 1. Inoculum Preparation: Prepare a standardized suspension of test microorganisms (e.g. bacteria, fungi) from active cultures.

[0165] 2. Exposure / Contact: Mix the test material (or its dilution) with the inoculum and incubate for specified contact times.

[0166] 3. Sampling & Neutralization: At defined intervals (e.g. 30 s, 1 min, etc.), withdraw aliquots and immediately neutralize the antimicrobial action (chemically or by dilution) to stop further killing.

[0167] 4. Enumeration of Survivors: Recover surviving microorganisms by plating on growth medium and incubate. Count colony forming units (CFU).

[0168] 5. Data Analysis: Calculate logw reduction or percentage reduction by comparing with initial microbial population (or a control). Plot kill vs time (killcurve).

[0169] Key Terms:

[0170] Neutralizer: agent or method used to inactivate the test material to prevent further killing after the sampling time.

[0171] Initial Population / Time Zero Control: the viable count immediately after inoculation (used as baseline).

[0172] Log Reduction: the reduction expressed in logw units (e.g. a 3-log reduction = 99.9% kill).

[0173] Strengths & Limitations:

[0174] Strengths:

[0175] Provides kinetic data (how fast kill occurs over time) rather than just endpoint.

[0176] Flexible: contact times, organisms, concentrations can be adapted. • More quantitative and reproducible than purely qualitative tests.

[0177] Limitations:

[0178] In vitro suspension test — may not reflect performance on surfaces or in complex matrices.

[0179] Sensitive to how inoculum and neutralization are handled; procedural variabilities affect results.

[0180] Because it’s a “best-case” exposure (direct contact in liquid), observed efficacy might overestimate real-world effect.Preservative Efficacy Test (USP <51>) (PET Test) OF THE COMPOSOTION

[0181] Purpose: To evaluate the effectiveness of antimicrobial preservatives in preventing the microbial growth in cosmetic or pharmaceutical formulations during storage and use, according to the present invention.

[0182] Microorganisms Used: Staphylococcus aureus (bacterium - Gram +), Escherichia coli (bacterium - Gram -), Pseudomonas aeruginosa (bacterium -Gram -), Candida albicans (yeast) and Aspergillus brasiliensis (mold)

[0183] Procedure: The product is inoculated with a known concentration of these microorganisms (usually 105— 106CFU / g or mL). Samples are stored at 20-25°C. Microbial counts are measured at specific time intervals — 7, 14, and 28 days

[0184] Acceptance Criteria (for cosmetics and topicals):

[0185] Bacteria: >2 log reduction by day 14 and no increase thereafter.

[0186] Yeast & Mold: No increase from initial count at any time point.

[0187] Interpretation: If microbial counts meet the required reduction criteria, the preservative system is considered effective.

[0188] The present invention offers a novel approach to preservation, addressing the limitations of traditional preservatives such as parabens and formaldehyde donors. Its multifunctional properties reduce the need for additional active ingredients, simplifying formulations and reducing costs. Its lowconcentration usage ensures minimal interference with the sensory properties of the final product.

[0189] The preservative composition comprising Undecylenic Acid makes this preservative an Ideal Choice for Natural Organic Formulations. The formulation blend provides additional benefits such as Anti-acne, Anti -dandruff, and Anti-plaque properties. The formulation blend is compatible with personal care and cosmetic formulations across skin care, skin cleansing, hair care, home care and oral care categories.

[0190] It is to be understood that the phraseology or terminology employed herein is for the purpose of description and not of limitation. Therefore, while the embodiments herein have been described in terms of preferred embodiments, those skilled in the art will recognize that the embodiments herein can be practiced with modification within the spirit and scope of the claims presented in the complete specification or non-provisional application.

Claims

Claims:We claim:

1. A preservative blend formulation having anti-microbial properties, comprises:a therapeutically active compound, wherein the therapeutically active compound is Chlorhexidine;undec- 10-enoic acid; andone or more aliphatic or aromatic acid.

2. The preservative blend formulation as claimed in claim 1, wherein the therapeutically active compound is present in a quantity of 54%-60% by weight.

3. The preservative blend formulation as claimed in claim 1, wherein the undecylenic acid is present in a quantity of 40%-46% by weight.

4. The preservative blend formulation as claimed in claim 1, wherein the one or more aliphatic or aromatic acid comprises benzoic acid, sorbic acid, salicylic acid, hydroxamic acid, dehydroacetic acid, and levulinic acid.

5. The preservative blend formulation as claimed in claim 1, wherein the one or more aliphatic or aromatic acid is present in a quantity of 2%-3% by weight.

6. The preservative blend formulation as claimed in claim 1, wherein the preservative works efficiently at a low concentration of up to 0.1% to 0.5%.

7. The preservative blend formulation as claimed in claim 1, wherein the preservative blend is in the form of a face cream, a Face wash, a hair mask, a wet wipes, and a mouth wash.

8. A method of synthesizing a preservative blend formulation having antimicrobial properties, comprises:adding a solvent into a reactor (101), wherein the solvent is alcohol; adding an undecylenic acid and an organic acid into the reactor while slowly purging nitrogen gas at room temperature to obtain a slurry (102);stirring the slurry for one hour (103);gradually adding chlorhexidine to the reactor to adjust the pH between 6.5 to 7.5 over a period to get a clear solution (104);cooling the solution to room temperature till crystals are formed (105); and separating the crystals by filtration (106).

9. The method as claimed in claim 8, wherein the organic acid is selected from the group consisting of benzoic acid, sorbic acid, salicylic acid, hydroxamic acid, dehydroacetic acid, and levulinic acid.

10. The method as claimed in claim 8, wherein the undecylenic acid is added in an amount of 40%-46% by weight.

11. The method as claimed in claim 8, wherein the organic acid is added in an amount of 2%-3% by weight.

12. The method as claimed in claim 8, wherein the chlorhexidine is added in a quantity of 54%-60% by weight.

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