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Transparent Personal Care And Cosmetic Products With Inorganic Active Ingredients In Micronized/Colloidal Form

Abstract: A transparent personal care composition is provided comprising pre-formed or in-situ generated metal particles that are able to provide cosmetic benefits despite reduced contact time. The present inventors have solved the problem of the prior art with the formulations of the present invention. A process for the preparation of the formulations with pre-formed or in-situ generated metal particle is also provided.

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Patent Information

Application #
Filing Date
27 August 2013
Publication Number
10/2015
Publication Type
INA
Invention Field
PHARMACEUTICALS
Status
Email
cal@patentindia.com
Parent Application
Patent Number
Legal Status
Grant Date
2018-10-09
Renewal Date

Applicants

ITC LIMITED
37, J. L. Nehru Road, Kolkata – 700 071, State of West Bengal, India.

Inventors

1. PANIGRAHI, Sudipa
ITC Limited, ITC R&D Centre, #3, 1st Main, Peenya Industrial Area, Phase 1, Bengaluru -560 058, India
2. MOHAMMED, Niyaz
ITC Limited, ITC R&D Centre, #3, 1st Main, Peenya Industrial Area, Phase 1, Bengaluru -560 058, India
3. RAMAMURTHI, Suresh
ITC Limited, ITC R&D Centre, #3, 1st Main, Peenya Industrial Area, Phase 1, Bengaluru -560 058, India
4. KRISHNAN, Venkat
ITC Limited, ITC R&D Centre, #3, 1st Main, Peenya Industrial Area, Phase 1, Bengaluru -560 058, India

Specification

CLIAMS:
1. A personal care composition comprising
a) active ingredient in an amount from 0.005% to 5% by wt.,
b) neutralizing base in an amount from 10% to 18% by wt., and
c) saturated fatty acids in an amount from 20% to 40% by wt.,
wherein the active ingredient is in-situ generated or pre-formed micronized/colloidal metal particle.

2. The personal care composition as claimed in claim 1, wherein size of the micronized/colloidal particles ranges from 1 nm to 1000 nm, more preferably from 10 nm to 200 nm.

3. The personal care composition as claimed in claim 1, wherein said active ingredient is selected from colloidal/micronized gold, colloidal/micronized silver, colloidal/micronized platinum, colloidal/micronized iron, colloidal/micronized copper.

4. The personal care composition as claimed in claim 1, wherein said neutralizing base is selected from sodium hydroxide, potassium hydroxide, magnesium hydroxide and ammonium hydroxide.

5. The personal care composition as claimed in claim 1, wherein said saturated fatty acid are selected from C10-C20 fatty acids such as lauric acid, myristic acid, palmitic acid, stearic acid and oleic acid.

6. The personal care composition as claimed in claim 1, wherein said metal particles are selected from gold and silver.

7. The personal care composition as claimed in claim 1, wherein said composition is adapted to provide anti-aging activity.

8. The personal care composition as claimed in claim 1, wherein said composition is adapted to provide anti-dandruff activity.

9. The personal care composition as claimed in claim 1, wherein said composition is adapted to provide anti-microbial activity.

10. A process for the preparation of personal care composition of claim 1 comprising:
a) Melting the mixture of fatty acids, optionally along with solvents at a temperature ranging from 70°C to 85°C °C under continuous stirring;
b) Mixing active ingredient to the molten mixture of step (a) under continuous stirring to obtain a mixture of active ingredients in fatty acids;
c) Neutralizing the mixture of active ingredients in fatty acids of step (b) with alkali solution under continuous stirring for in-situ generation of saponified colloidal metal particles; and
d) Optionally adding surfactants, colourants and fragrances to the in situ generated saponified colloidal metal particles of step (c) and molding the same to obtain personal care composition comprising in-situ generated colloidal metal particles.

11. A process for the preparation of active ingredient of claim 1 comprising
a) Preparation of stock solution of active ingredient in water;
b) Addition of reducing agent drop-wise to the active ingredient solution of step (a) under continuous stirring condition to form a reduced solution;
c) Mixing the reduced solution of step (b) for 5 to 60 seconds minutes under continuous stirring for complete generation of a solution of colloidal / micronized metal particles; and
d) Storing the solution of colloidal / micronized metal particles of step (c) in the dark before adding it to the personal care formulation.

12. The process for the preparation of active ingredient as claimed in claim 11, wherein said stock solution is a precursor of active ingredient in water.

13. The process for the preparation of active ingredient as claimed in claim 11, wherein said reducing agent comprises of glucose, sodium borohydride, sucrose and fructose.

14. The process for the preparation of active ingredient as claimed in claim 12, wherein said stock solution comprises of metal particles.

15. The process for the preparation of active ingredient as claimed in claim 14, wherein said metal particles are present in an amount ranging from 0.005% to 5% by wt.

16. The process for the preparation of active ingredient as claimed in claim 13, wherein the amount of reducing agent is approximately four times the concentration of said metal particles in said stock solution.
,TagSPECI:
FIELD OF THE INVENTION

The present invention relates to personal care compositions that provide excellent skin benefits despite an extremely less contact time. More specifically it relates to personal care composition that delivers anti acne, antimicrobial and antidandruff benefits to skin and scalp. Even more specifically the invention relates to personal care compositions comprising pre-formed or in-situ generated metal particles and process for preparation thereof. Most specifically the invention relates to transparent personal care compositions comprising pre-formed or in-situ generated metal particles and process for preparation thereof.

BACKGROUND AND THE PRIOR ART

Transparent cleansing products are made of glycerin, and are partly soap and partly solvent. Sodium hydroxide generates soap crystals, and makes it opaque. In order to make it transparent, the soap has to be dissolved in enough solvent to make the crystals so small that light passes freely through, making the soap look transparent. Any foreign particle can induce crystals to grow and affect the transparency. Incorporation of inorganic active ingredients into the soap matrix without affecting the transparency is challenge to the product developer.

It is always a technical challenge to provide the skin benefits through cleansing products due to its extremely less contact time. Precious metals e.g. gold, silver and copper have attracted people for several years because of its skin benefits. Because of its proven therapeutic use of gold and silver it is a demand from the consumer to incorporate these active ingredients into the cleansing products. Addition of these as a dust to the product can affect the sensory and eventually will settle down making it heterogeneous. This will drastically affect the transparency of the product. Above all because of its larger size these particles could not provide any skin benefits directly.

EP 1364639 A2 discloses glasses, color glass, glass ceramics, ceramics, glass powders, color glass powders, glass ceramic powders, ceramic powders, or composite materials comprising glass or glass ceramics or ceramic powders or mixtures of glass, ceramic and glass ceramic powders. These can be used in different cosmetic formulations for cosmetic products such as transparent pearly lotion, gel cologne with sparkles, pearlescent waterproof sun cream, bronze self tanning cream, sunscreen cream, pearl bronze/copper suntan cream, Icy gel toothpaste, face mask for oily skin, etc. Further EP 1364639 also discloses a cosmetic formulation with ceramic glass particles that are used in composite material comprising nano-particle gold, silver etc.

Drawbacks of nano-particles are that they are very prone aggregation or agglomeration due to the very high surface to volume ratio. The aggregation also depends on the chemical and physical environment around the particles.

EP 1914264 A1 discloses a surface-treated powder, more specifically to a novel surface-treated powder prepared by treating (coating) the surface of a powder (particle) comprising a silicone resin and/or an organic powder with a specific hydrophilizing agent. Further, it mentions that the use of the surface-treated powder or the use of the dispersion can provide further a cosmetic excellent in dispersibility and dispersion stability and further in re-dispersibility and dispersion stability with lapse of time and smooth feeling. Gold powder and silver powder are few examples of the inorganic powders used in cosmetics as colorants, screening agents, ultraviolet shielding agents. Example 14 and 15 of EP 1914264 disclose a method for preparation of cosmetic where the appearance of the cosmetic composition is semi transparent.

US 20080057136 A1 relates to an antimicrobial composition that is used for disinfecting. The antimicrobial compositions comprise a chelating metal complex compound with a monodentate bidentate or polydentate ligand that exhibits affinity to hydrogen ion, an ionogenic surfactant, and a solvent. The metal used in the composition is selected from the group consisting of copper, zinc, mercury, chromium, manganese, nickel, cadmium, arsenic, cobalt, aluminum, lead, selenium, platinum, gold, titanium, tin etc.

WO2006118940 relates to compositions comprising one or more discrete particle aggregates and/or agglomerates, and methods of using said compositions for application onto keratin fibers, preferably hair. WO2006118940 further recites that the reduced size of the discrete particle aggregates and/or agglomerates can deliver the defined benefits. The particle aggregates and agglomerates further comprise a chromophoric material selected from the group consisting of: metal oxides, aluminum, ceramic, cerium, copper, diamond, gold, graphite, hasteloy, indium, platinum, silicon, silver, talc, tin, zinc and zirconium carbon black, gold colloid, silver colloid, metal nano-composites, non-metal nano-composites, doped metal oxides, synthetic or naturally occurring melanin (or derivatives), organic pigments and mixtures thereof. Further WO2006118940 also provides shine, hold, body, sheen, volume, stiffness, weight, curl and condition in an efficient manner to the hair.

A 100% gold transparent soap is disclosed on http://www.chemkind.com/chemicals-p_2086679_100-gold-transparent-soap.htm. The features listed on the product provide information that recites that the product provides detoxifying activity of pure gold, promotes blood circulation by removing skin impurities, and thus solves skin troubles. Its main ingredients are amino acids and coconut extracts and sugarcane. The other essential ingredient include natural moisturizing factors such as albumin and hyaluronic acid, which reduces blackheads, reduces pore size and improves skins elasticity, keeping it smooth, soft and supple. It is a weak acid in pH value and this mixture of fruit acids are effective for skin whitening and keratin decomposition. It also causes less skin irritation. Due to its superior biodegradation ability, it leaves almost no remnants from skin and enables gold to easily penetrate into skin. Further it recites that the product contains 100% 24k Gold. It is very clear and transparent and has a pH of 5.5 amino acid base which is the same as human skin.

However the product named 100% gold transparent soap is a facial pack and not a soap and also the composition of facial pack is different.

Incorporating some inorganic material in a transparent formulation is always a challenging task as a small change in the formulation can affect the transparency and make it translucent or opaque. All the prior arts disclose the use of the composite materials mainly in opaque system. Transparent systems are always appealing to the consumers compared to the translucent and opaque system.

OBJECTS OF THE INVENTION

It is an object of the invention to overcome the drawbacks of the prior art.

It is another object of the invention to provide personal care compositions that provide excellent skin benefits within extremely less contact time.

It is yet another object of the invention to provide transparent personal care cleansing compositions that provide excellent skin benefits within extremely less contact time.

It is still another object of the present invention to provide transparent personal care and cosmetic products with inorganic active ingredients in micronized/colloidal form.

It is further the object of the present invention to provide a process for the preparation of the transparent personal care and cosmetic products with inorganic active ingredients in micronized/colloidal form.

SUMMARY OF THE PRESENT INVENTION

An embodiment of the present invention provides a personal care composition comprising

a) active ingredient in an amount from 0.005% to 5% by wt.,
b) neutralizing base in an amount from 10% to 18% by wt., and
c) saturated fatty acids in an amount from 20% to 40% by wt.,

wherein the active ingredient is in-situ generated or pre-formed micronized/colloidal metal particle.

Another embodiment of the present invention provides a process for the preparation of personal care composition comprising:
a. melting the mixture of fatty acids, optionally along with solvents at a temperature ranging from 70°C to 85°C °C under continuous stirring;
b. mixing active ingredient to the molten mixture of step (a) under continuous stirring to obtain a mixture of active ingredients in fatty acids;
c. neutralizing the mixture of active ingredients in fatty acids of step (b) with alkali solution under continuous stirring for in-situ generation of saponified colloidal metal particles; and
d. optionally adding surfactants, colourants, fragrances to the in situ generated saponified colloidal metal particles of step (c) and molding the same to obtain personal care composition comprising in-situ generated colloidal metal particles.
Yet another embodiment of the present invention provides process of preparation of the active ingredient of claim 1 comprising the steps of:

a) Preparation of stock solution of active ingredient in water;
b) Addition of reducing agent drop-wise to the active ingredient solution of step (a) under continuous stirring condition to form a reduced solution;
c) Mixing the reduced solution of step (b) for 5 to 60 seconds minutes under continuous stirring for complete generation of a solution of colloidal / micronized metal particles; and
d) Storing the solution of colloidal / micronized metal particles of step (c) in the dark before adding it to the personal care formulation.

DETAILED DESCRIPTION OF THE PRESENT INVENTION

The present inventors have found that incorporation of metal particles like gold and silver in micronized/colloidal form into the product provides several skin benefits such as anti-acne, anti-microbial, anti-dandruff, anti-aging etc. It also helps to maintain the youthful skin.

In an embodiment of the present invention there is provided a transparent personal care composition comprising:

a) active ingredient in an amount of from 0.005% to 5% by wt.;
b) neutralizing base in an amount of from 10% to 18% by wt.; and
c) saturated fatty acids in an amount of from 20% to 40% by wt.

wherein the active ingredient is in-situ generated or pre-formed micronized/colloidal form of metal particles.

The personal cleansing composition kills 96% of Staphylococcus aureus strain number MTCC 96 within 1 minute of contact and 99.99% within 30 minute of contact as compared to saline (untreated control) confirming its anti-microbial activity. Further, the personal care formulation provides a zone of inhibition of 10-15 mm against Mallasezia Furfur strain number MTCC 1374 confirming its anti-dandruff activity. The personal care formulation kills 10% of Propinibacterium acnes strain number 1951 MTCC within 1 minute of their contact and killed 58% Propinibacterium acnes strain number 1951 MTCC within 30 minute of their contact confirming its anti-acne activity.

The expression “in-situ generated” as used herein is meant by when colloidal metal particles were generated during the batch through the addition of appropriate metal precursors.

The expression “pre-formed micronized/colloidal form” as used herein is meant by when colloidal metal particles were synthesized separately and added to the batch.

The expression “active ingredient” as used herein refers to metal particles, in their various states and forms (such as crystalline, amorphous, colloidal, micronized), derivatives and combinations thereof; and to precursors of these metal particles.

The expression “molding” as used herein refers to process of giving shape to a given preparation. The term is synonymous to casting for semisolid / solid preparations and to pouring into containers for liquid and/or semisolid compositions; as applicable.

The size of the micronized/colloidal particles ranges from 1 nm to 1000 nm, more preferably from 10 nm to 200 nm.

The active ingredients used in the transparent soap bar with particles like gold and silver can be selected from colloidal/micronized gold, colloidal/micronized silver, colloidal/micronized platinum, colloidal/micronized iron, colloidal/micronized copper, derivatives and precursors to colloidal/micronized gold, colloidal/micronized silver, colloidal/micronized platinum, colloidal/micronized iron, colloidal/micronized copper, such as Chloroauric Acid, Gold(III) chloride hydrate, Gold(III) chloride, Gold(I) chloride, Chloro(triphenylphosphine) Gold(I), Potassium Gold(III) chloride, Gold(III) bromide, Gold(I) sulfide, Gold(III) sulfide, silver nitrate, silver chloride, silver acetate, silver sulfate, silver(I) fluoride, silver acetylacetonate, silver perchlorate, silver iodide, silver bromide, silver sulfide, silver lactate, silver citrate hydrate etc. The amount of the active ingredient ranges from 5.0% to 0.005% by wt., preferably from 0.5% to 0.05% by wt.

The neutralizing base used in the transparent soap bar of the present invention can be selected from sodium hydroxide, potassium hydroxide, magnesium hydroxide, ammonium hydroxide etc. The preferable base for the preparation of transparent soap bar of the present invention is sodium hydroxide and potassium hydroxide. The amount of the base ranges from 10 to 18% by wt, preferably from 13 to 16% by wt.

The saturated fatty acids used in the transparent soap bar of the present invention can be selected from C10-C20 fatty acids such as lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid and the like. The preferable saturated fatty acids for the preparation of transparent soap bar of the present invention are lauric acid, myristic acid, palmitic acid, stearic acid. The amount of the saturated fatty acids ranges from 10 to 40% by wt, preferably from 20 to 30% by wt.

The transparent soap bar of the present invention may further comprise solvent(s) selected but not limited to from propylene glycol, butylenes glycol, sorbitol, glycerine, PEG 400, sucrose etc. The preferable solvents for the preparation of transparent soap bar of the present invention are propylene glycol, glycerine, sorbitol, sucrose and PEG 400. The amount of the solvent ranges from 30 to 50%, preferably from 30 to 40% by wt.

The transparent soap bar of the present invention may further comprise chelating agent selected from Ethylenediamminetetraacetic acid (EDTA), disodium EDTA, tetrasodium EDTA, etc. The preferable chelating agents for the preparation of transparent soap bar of the present invention are tetrasodium EDTA, disodium EDTA etc. The amount of the chelating agent ranges from 0.01 to 1% by wt, preferably from 0.3 to 0.6% by wt.

The transparent soap bar of the present invention may further comprise binder selected from sodium chloride, potassium chloride, magnesium chloride etc. The preferable binder for the preparation of transparent soap bar of the present invention is sodium chloride and potassium chloride. The amount of the binder ranges from 0.1 to 2% by wt, preferably from 0.3 to 0.8% by wt.

The transparent soap bar of the present invention may further comprise surfactant(s) selected from anionic, non-ionic and amphoteric such as sodium lauryl ether sulfate, sodium lauryl sulfate, cocamidopropyl betaine, decyl glucoside, sodium cocoyl isethionate and the like. The preferable surfactant for the preparation of transparent soap bar of the present invention is sodium lauryl ether sulfate, sodium lauryl sulfate, cocamidopropyl betaine. The amount of the surfactant ranges from 0.5 to 20% by wt, preferably from 5 to 15% by wt.

The composition additionally comprises fragrance ranging from 0.5% to 1.5% by wt.

The present invention discloses personal care compositions comprising both in-situ generated or pre-formed micronized/colloidal metal particles. The invention also discloses process for he preparation of personal care compositions comprising pre-formed micronized/colloidal metal particles. The invention further discloses process for the preparation of personal care compositions comprising in-situ generated micronized/colloidal metal particles.

Still further the invention discloses a process for the in-situ generation of the micronized/colloidal metal particles. The generation in-situ micronized/colloidal form of the actives is during the process of batch making of the personal care formulations. The advantage of the same is that an extra step of material preparation is avoided.

Advantages of in-situ micronized/colloidal particles of present invention

Ø By generating the micronized/colloidal particles in-situ from their corresponding metal salts one extra step of could be avoided.
Ø Storing of the micronized/colloidal particles can also be avoided if the micronized/colloidal are generated in-situ.
Ø The preformed particles could also undergo agglomeration if stored for long time while generating the micronized/colloidal in-situ this problem could also be avoided.

The pre-formed colloidal metal particles are incorporated into the personal care composition or can be generated in-situ.

The process of incorporation of inorganic active ingredients e.g. gold, silver, copper etc. in its micronized/colloidal form into the personal care products such as soap, shampoo, body wash, face wash, lotions, creams etc. The particle of choice could be either generated in-situ or could be added separately during the process without affecting its transparency and other sensorial aspects. The particles are distributed well through the product and make the mixture homogeneous.

The present invention discloses both in-situ generated and pre-formed micronized/colloidal metal particles. In-situ generation of the metal particles is one of the important inventive steps along with other inventive steps.

In-situ generation of the micronized/colloidal particles is an additional inventive feature of the present invention. The micronized / colloidal metal particles when used in the composition of the current invention provide an effective transparent personal care / personal cleansing composition.

PERSONAL CARE COMPOSITIONS

The personal care compositions of the present invention are transparent with less sodium hydroxide and more solvent containing colloidal gold particles. Soap free skin cleansing formulation containing surfactants are also transparent in nature. Skin care products such as hydrogel etc. are also transparent. Hair care formulations such as shampoo, conditioner, serum, hair gels are transparent too. In may be understood that these formulations may be made opaque by addition of opacifiers, if need be. Such opaque formulations may be considered a part of this invention too.

Addition of sodium hydroxide is required to generate the soap from their corresponding fatty acids. For hair care and skin care formulation small amount of sodium hydroxide solution is not required if the micronized/colloidal metal particles is used.

Process for the preparation of the pre-formed metal particles prior to the incorporation in the personal care formulation comprises steps of:

a) Preparation of stock solution of active ingredient in water
b) Addition of reducing agent drop-wise to the active ingredient solution of step (a) under continuous stirring condition to form a reduced solution
c) Mixing the reduced solution of step (b) for 5 to 60 seconds minutes under continuous stirring for complete generation of a solution of colloidal / micronized metal particles
d) Storing the solution of colloidal / micronized metal particles of step (c) in the dark before adding it to the personal care formulation.

Stock solution refers to a solution of active ingredients, i.e. precursors to metal particles, in water. The concentration of stock solution can vary and as per requirement, a diluted solution of active ingredient can be prepared from stock solution. The amount of stock solution required in the composition varies depending on the concentration of metal particles required in the final product. The concentration of the metal particles ranges from about 0.005% to 5% by wt.

Reducing agent referred to in the second step of preparation of pre-formed metal particles refers to any chemical which can reduce the metal from different its oxidative state to zero oxidation state for example glucose, sodium borohydride, sucrose and fructose. The amount of reducing agent depends on the concentration of stock solution and is approximately more than four times higher than the concentration of metal precursor in stock solution.

INCORPORATION OF PRE-FORMED COLLOIDAL METAL PARTICLES IN THE PERSONAL CARE FORMULATION

The incorporation of the pre-formed micronized/colloidal metal particles helps to provide multiple skin and hair benefits e.g. skin benefits such as anti-acne, anti-microbial, anti-dandruff, anti-aging etc.

The personal care formulation with the active ingredient (colloidal/micronized metal particles) killed 10% of Propinibacterium acnes strain number 1951 MTCC within 1 minute of their contact and killed 58% Propinibacterium acnes strain number 1951 MTCC within 30 minute of their contact as compared to the formulation without it, which confirms its anti-acne activity.

The personal care formulation with active ingredient (colloidal/micronized metal particles) killed 96% of Staphylococcus aureus strain number MTCC 96 within 1 minute of contact and 99.99% within 30 minute of contact as compared to the personal care formulation without it which confirms its anti-microbial activity.

The personal care formulation with active ingredient (colloidal/micronized metal particles) provides anti-dandruff activity against Mallasezia Furfur strain number MTCC 1374. The zone of inhibition for the anti-dandruff activity was found to be 10-15 mm.

Further we note that one of the features of the present invention is to stabilize the particles within the personal care product matrix and make it homogeneous. The micronized/colloidal metal particles are stabilized by the fatty acids, surfactants and solvents present in the formulations.

Pre-formed micronized/colloidal metal particles are added into the personal care composition last along with fragrance.

IN-SITU GENERATION OF MICRONIZED/COLLOIDAL METAL PARTICLES

The in-situ generation of micronized/colloidal metal particles comprises

a. melting the mixture of fatty acids, optionally along with solvents at a temperature ranging from 70°C to 85°C °C;
b. mixing active ingredient to the molten mixture of step 1 under continuous stirring to obtain a mixture of active ingredients in fatty acids;
c. neutralizing the mixture of active ingredients in fatty acids of step 2 with alkali solution under continuous stirring for in-situ generation of saponified colloidal metal particles; and
d. optionally adding surfactants, colourants, fragrances to the in situ generated saponified colloidal metal particles of step 3 and molding the same to obtain transparent soap bar containing in-situ generated colloidal metal particles.

In the above process, mixing step is carried out under continuous stirring for 2 to 5 minutes.

Step (3) helps in the generation of the in-situ micronized/colloidal metal particles and for the process of saponification.

The active ingredients as used in the in-situ generation of micronized/colloidal metal particles of the present invention include but are not limited to Gold(III) chloride hydrate, Gold(III) chloride, Gold(I) chloride, Chloro (triphenylphosphine) Gold(I), Potassium Gold(III) chloride, Gold(III) bromide, Gold(I) sulfide, Gold(III) sulfide, silver nitrate, silver chloride, silver acetate, silver sulfate, silver(I) fluoride, silver acetylacetonate, silver perchlorate, silver iodide, silver bromide, silver sulfide, silver lactate, silver citrate hydrate and combinations thereof in an amount ranging from 0.0001 to 1% by wt., preferably from 0.01 to 0.1% by wt.

Saponification in the meaning of the present invention is defined as “neutralization of fatty acids by alkali e.g. sodium hydroxide, potassium hydroxide, ammonium hydroxide etc. to generate soap”.

The ‘personal care compositions’ according to present invention that use in-situ generated micronized/colloidal metal particles can be soap, shampoo, conditioner, face wash, body wash, shower gel, hair gel, body lotion, cream etc.

The present invention is now illustrated by way of non-limiting examples. Experiments have been conducted to illustrate the importance of in situ micronized metal oxide particles in the transparent personal care and cosmetic products.

Example 1

Transparent soap formulation comprising pre-formed colloidal gold particles

Table 1
S No Materials Function w/w (%)
1 Propylene Glycol Solvent 21.7
2 Glycerine Solvent 5
3 Tetrasodium EDTA Chelating Agent 0.05
4 Sodium Hydroxide (48%) Base 12.1
5 Sodium Chloride Binder 0.3
6 Perfume Fragrance 0.88
7 Sorbitol Solvent 16.5
8 (C12-C14) fatty Acids Saturated Fatty Acids 31.47
9 Sodium Laureth Sulfate 1-EO Surfactant 7
10 CAPB Surfactant 4.0
11 Colloidal Gold Active Ingredient 1.0

Example 2

Synthesis of colloidal/micronized gold or metal nanoparticles and incorporation of the pre-formed colloidal gold particles in the transparent soap formulation

The process of preparation of colloidal gold particles comprised of the following steps

Step 1: Preparation of colloidal gold
i. In a 100 mL beaker weight 5 gm of D (+) Glucose,
ii. Dissolve the D(+) Glucose in 48 mL of water and mix well to get a homogeneous solution,
iii. Mix 2 mL of 10-2M HAuCl4 solution to the solution obtained from step ii and mix well.
iv. Add 100 µL of 1M KOH solution drop-wise to the mixture obtained from step iii under continuous stirring condition,
v. The colour of the mixture will turn from very light yellow to purple colour indicating the formation of colloidal gold in water,
vi. Mix the solution for 10 minute for complete conversion of HAuCl4 to colloidal gold in water,
vii. Store the colloidal gold particles in dark to be used in transparent soap formulation.

Step 2: Incorporation of colloidal gold particles in transparent soap formulation

i. Mixing hot melting of soap mass comprising free fatty acids, additives, solvents selected from glycerin, sorbitol, isopropyl alcohol, propylene glycol, and water at moderate temperature (70°C to 85°C);
ii. neutralizing the mixture obtained from step (i) with alkali selected from sodium hydroxide, potassium hydroxide, lithium hydroxide, calcium hydroxide, magnesium hydroxide to generate the fatty acid soap at moderate temperature (70°C to 85°C)
iii. Addition of surfactants comprising but not limited to Surfactants according to the present invention can be anionic, non-ionic and amphoteric such as sodium laureth sulphate, cocamidopropyl betaine, sodium cocoyl isethionate and the like.
iv. Addition of colloidal gold at lower temperature (40°C to 50°C) under continuous mixing
v. Addition of fragrance at lower temperature (40°C to 50°C) under continuous mixing
vi. casting the mixture of step (v) at different temperature (-5°C to 80°C) into the mould to get the soap bar of desired size and shape.

Example 3

Personal care formulation comprising in-situ generation of colloidal metal particles
Table 2
S No Materials Function w/w (%)
1 Propylene Glycol Solvent 21.7
2 Glycerine Solvent 5.5
3 Sucrose Binder/Reducing agent 0.5
4 Tetrasodium EDTA Chelating Agent 0.05
5 Sodium Hydroxide (48%) Base 12.1
6 Sodium Chloride Binder 0.3
7 Perfume Fragrance 0.83
8 Sorbitol Solvent 16.5
9 (C12-C14) fatty Acids Saturated Fatty Acids 31.47
10 Sodium Laureth Sulfate 1-EO Surfactant 7.0
11 CAPB Surfactant 4.0
12 Chloroauric Acid Active Ingredient 0.05

Example 4
Synthesis of in-situ colloidal metal particles

The process for the preparation of in-situ colloidal metal particles in the personal care formulation comprised of the following steps

i. Mixing hot melting of soap mass comprising free fatty acids, additives, sucrose, solvents selected from glycerin, sorbitol, isopropyl alcohol, propylene glycol, and water at moderate temperature (70°C to 85°C);
ii. Addition of Choloroauric acid to the hot melt and mixing at moderate temperature (70°C to 85°C);
iii. neutralizing the mixture obtained from step (ii) with alkali selected from sodium hydroxide, potassium hydroxide, lithium hydroxide, calcium hydroxide, magnesium hydroxide for the in-situ generation of colloidal gold particles in the in the hot melt of fatty acid soap at moderate temperature (70°C to 85°C)
iv. Addition of surfactants comprising but not limited to Surfactants according to the present invention can be anionic, non-ionic and amphoteric such as sodium laureth sulphate, cocamidopropyl betaine, sodium cocoyl isethionate and the like at moderate temperature (60°C to 70°C).
v. Addition of fragrance at temperature (40°C to 50°C) under continuous mixing
vi. casting the mixture of step (v) at different temperature (-5°C to 80°C) into the mould to get the soap bar of desired size and shape to get the transparent soap containing in-situ generated colloidal gold particles.

Example 5
Transparent shampoo formulation comprising colloidal silver particles is given below:
Table 3

S No Ingredient w/w (%)
1 Ammonium Lauryl Sulfate 20
2 Ammonium Laureth Sulfate 21
3 Cocamidiopropyl Betaine 6
4 Decyl Glucoside 11
5 DMDM Hydantoin 0.3
6 PEG 400 5
7 Deionised Water 32.5
8 Cocamide DEA 2.0
9 Colloidal Silver 1.0
10 Fragrance 0.6
11 Hydroxypropyl Guar HydroxypropyltrimoniumChloride 0.3
12 Disodium EDTA 0.3
13 Citric Acid q.s.

Process:

Step 1: Mix Ammonium lauryl sulfate, disodium EDTA and 22.5 % water at heat it to 70-75°C until uniform.

Step 2: In a separate vessel mix ammonium laureth sulfate, cocamidopropyl betaine and cocamide DEA with mixing.

Step 3: Add the mixture obtained from step 1 to the mixture obtained from step 2 under mixing.

Step 4: In a separate vessel mix hydroxypropyl Guar hydropropyltriamonium chloride in the remaining water and mix it properly.

Step 5: Add the mixture obtained from step 4 to the mixture obtained from step 3 properly and cool it to 40°C.

Step 6: Add DMDM hydantoin to the mixture obtained from Step 5.

Step 7: Add colloidal silver to the mixture obtained from step 6 and mix properly until homogeneous.

Step 8: Adjust pH to 6.5 with Citric acid.

Step 9: Add fragrance and mix well.

Example 6

Transparent hair gel formulation comprising colloidal silver particles is given below

Table 4

SI No Ingredients w/w (%)
1 Dimethicone 2.5
2 Cyclopentasiloxane 82.4
3 Fragrance 0.1
4 Colloidal Silver 2.0
5 C12-C15 Alkyl Benzoate 3.0
6 PEG 400 10

Process:
Mix all the ingredients together until homogeneous.

Example 7

The skin care formulation with 2% active ingredient (colloidal/micronized metal particles) killed 10% of Propinibacterium acnes strain number 1951 MTCC within 1 minute of their contact and killed 58% Propinibacterium acnes strain number 1951 MTCC within 30 minute of their contact of as compared to saline (untreated control).

The skin care formulation with 2% active ingredient (colloidal/micronized metal particles) killed 96% of Staphylococcus aureus strain number MTCC 96 within 1 minute of contact and 99.99% within 30 minute of contact as compared to saline (untreated control) which confirms its anti-microbial activity.

Example 8

The skin care formulation with 2% active ingredient(colloidal/micronized metal particles) killed 96% of Staphylococcus aureus strain number MTCC 96 within 1 minute of contact and 99.99% within 30 minute of contact as compared to saline (untreated control) which confirms its anti-microbial activity.

The personal care formulation with active ingredient (colloidal/micronized metal particles) provides anti-dandruff activity against Mallasezia Furfur strain number MTCC 1374.The zone of inhibition for the anti-dandruff activity was found to be 10-15 mm.

Documents

Orders

Section Controller Decision Date

Application Documents

# Name Date
1 988-KOL-2013-RELEVANT DOCUMENTS [30-09-2023(online)].pdf 2023-09-30
1 GPA of ITC limited.pdf 2013-09-03
2 988-KOL-2013-RELEVANT DOCUMENTS [27-09-2022(online)].pdf 2022-09-27
2 FORM 3.pdf 2013-09-03
3 FORM 2 & Complete Specification.pdf 2013-09-03
3 988-KOL-2013-RELEVANT DOCUMENTS [25-09-2021(online)].pdf 2021-09-25
4 988-KOL-2013-RELEVANT DOCUMENTS [25-03-2020(online)].pdf 2020-03-25
4 988-KOL-2013-(18-09-2013)-FORM-1.pdf 2013-09-18
5 988-KOL-2013-FORM 4 [29-06-2019(online)].pdf 2019-06-29
5 988-KOL-2013-(18-09-2013)-CORRESPONDENCE.pdf 2013-09-18
6 988-KOL-2013-RELEVANT DOCUMENTS [31-03-2019(online)].pdf 2019-03-31
6 988-KOL-2013-FORM-18.pdf 2013-10-08
7 988-KOL-2013-IntimationOfGrant09-10-2018.pdf 2018-10-09
7 988-KOL-2013-FER.pdf 2017-10-13
8 988-KOL-2013-PatentCertificate09-10-2018.pdf 2018-10-09
8 988-KOL-2013-FER_SER_REPLY [13-04-2018(online)].pdf 2018-04-13
9 988-KOL-2013-CLAIMS [13-04-2018(online)].pdf 2018-04-13
9 988-KOL-2013-Written submissions and relevant documents (MANDATORY) [28-08-2018(online)].pdf 2018-08-28
10 988-KOL-2013-ExtendedHearingNoticeLetter_13Aug2018.pdf 2018-07-19
10 988-KOL-2013-HearingNoticeLetter.pdf 2018-06-18
11 988-KOL-2013-REQUEST FOR ADJOURNMENT OF HEARING UNDER RULE 129A [09-07-2018(online)].pdf 2018-07-09
12 988-KOL-2013-ExtendedHearingNoticeLetter_13Aug2018.pdf 2018-07-19
12 988-KOL-2013-HearingNoticeLetter.pdf 2018-06-18
13 988-KOL-2013-CLAIMS [13-04-2018(online)].pdf 2018-04-13
13 988-KOL-2013-Written submissions and relevant documents (MANDATORY) [28-08-2018(online)].pdf 2018-08-28
14 988-KOL-2013-FER_SER_REPLY [13-04-2018(online)].pdf 2018-04-13
14 988-KOL-2013-PatentCertificate09-10-2018.pdf 2018-10-09
15 988-KOL-2013-FER.pdf 2017-10-13
15 988-KOL-2013-IntimationOfGrant09-10-2018.pdf 2018-10-09
16 988-KOL-2013-FORM-18.pdf 2013-10-08
16 988-KOL-2013-RELEVANT DOCUMENTS [31-03-2019(online)].pdf 2019-03-31
17 988-KOL-2013-(18-09-2013)-CORRESPONDENCE.pdf 2013-09-18
17 988-KOL-2013-FORM 4 [29-06-2019(online)].pdf 2019-06-29
18 988-KOL-2013-(18-09-2013)-FORM-1.pdf 2013-09-18
18 988-KOL-2013-RELEVANT DOCUMENTS [25-03-2020(online)].pdf 2020-03-25
19 FORM 2 & Complete Specification.pdf 2013-09-03
19 988-KOL-2013-RELEVANT DOCUMENTS [25-09-2021(online)].pdf 2021-09-25
20 FORM 3.pdf 2013-09-03
20 988-KOL-2013-RELEVANT DOCUMENTS [27-09-2022(online)].pdf 2022-09-27
21 GPA of ITC limited.pdf 2013-09-03
21 988-KOL-2013-RELEVANT DOCUMENTS [30-09-2023(online)].pdf 2023-09-30

Search Strategy

1 988KOL2013Searchstrategy_11-10-2017.pdf
1 DisplayDocumentDuringFER_11-10-2017.pdf
2 988KOL2013Searchstrategy_11-10-2017.pdf
2 DisplayDocumentDuringFER_11-10-2017.pdf

ERegister / Renewals

3rd: 01 Jul 2019

From 27/08/2015 - To 27/08/2016

4th: 01 Jul 2019

From 27/08/2016 - To 27/08/2017

5th: 01 Jul 2019

From 27/08/2017 - To 27/08/2018

6th: 01 Jul 2019

From 27/08/2018 - To 27/08/2019

7th: 01 Jul 2019

From 27/08/2019 - To 27/08/2020

8th: 31 Oct 2019

From 27/08/2020 - To 27/08/2021

9th: 18 Mar 2021

From 27/08/2021 - To 27/08/2022

10th: 16 Dec 2021

From 27/08/2022 - To 27/08/2023

11th: 26 Aug 2023

From 27/08/2023 - To 27/08/2024

12th: 22 Aug 2024

From 27/08/2024 - To 27/08/2025

13th: 02 Jan 2025

From 27/08/2025 - To 27/08/2026

14th: 02 Jan 2025

From 27/08/2026 - To 27/08/2027

15th: 02 Jan 2025

From 27/08/2027 - To 27/08/2028

16th: 02 Jan 2025

From 27/08/2028 - To 27/08/2029

17th: 02 Jan 2025

From 27/08/2029 - To 27/08/2030

18th: 02 Jan 2025

From 27/08/2030 - To 27/08/2031

19th: 02 Jan 2025

From 27/08/2031 - To 27/08/2032

20th: 02 Jan 2025

From 27/08/2032 - To 27/08/2033