Title of Invention

IMPROVED COSMETIC COMPOSITION FOR TOPICAL APPLICATION FOR DEODRANT BENEFIT

Abstract A composition for topical application comprising (a) 0.5 - 40% of a mixed metal oxide having the general formula (M)a(N)bOc wherein M is a group II divalent cation not having antimicrobial property and N is a group III trivalent cation and a has a value in the range of 0.3 to 0.9, b has a value in the range of 0.1 to 0.3 and c =1 (b) 10- 99.5% of a topically acceptable carrier.
Full Text FORM-2
THE PATENTS ACT, 1970
(39 of 1970)
&
The Patents Rules, 2003
COMPLETE SPECIFICATION
(See Section 10 and Rule 13)
IMPROVED COSMETIC COMPOSITION
FOR TOPICATION FOR DEODRANT
DENEFIT
HINDUSTAN LEVER LIMITED, a company incorporated under the Indian Companies Act, 1913 and having its registered office at Hindustan Lever House, 165/166, Backbay Reclamation, Mumbai -400 020, Maharashtra, India
The following specification particularly describes the invention and the manner in which it is to be performed.

TECHNICAL FIELD
The invention relates to a synergistic composition for topical application for improved deodourancy benefit. This invention particularly relates to a powder composition for controlling axillary malodour.
BACKGROUND AND PRIOR ART
There is a lot of information of the ways in which products have been formulated to prevent or minimize body odour. Several products rely on use of perfumery compounds that mask the malodour produced by the body. The concentration and impact of these perfumery compounds is so strong and long-lasting that the off-odours produced by the body is not apparent to the nose for a long time after topical application of the product. Some investigators have tried to tackle the problem by controlling the growth or killing the microorganisms which reside on the skin. These microorganisms feed on the secretions produced by the human body on the skin and the by-products produced by the micoorganims produce the malodour. Thus, by controlling the growth/killing of these microorganisms, the malodour produced on the human skin is controlled. Several materials which act as bactericidal or bacteriostatic agents are known and have been incorporated in malodour reducing cosmetic compositions for topical application. Deodourant compositions in powder form e.g. talcum powders, in stick form e.g. roll-on deodourant sticks, in cream form and in spray form are known and widely used.
EP 0737711 B1 (Kyowa, 2000) describes a ultraviolet protective agent which also has sterilising and deodourising properties which comprises a mixed metal oxide comprising zinc and additionally a divalent metal cation and a trivalent metal cation.
WO94/14409 (Unilever, 1994) describes a deodourant composition for topical application to human skin e.g. underarm which contain as an active agent a layered double hydroxide of a general formula comprising zinc and aluminium.


EP 0368420 B1 (Unilever, 1989) describes an oral composition for removing oral bacteria, comprising from 0.01 to 30% of a layered hydrotalcite material which comprises a divalent cation and a trivalent/tetravalent cation. In this publication the preferred divalent cations have bacteriostatic properties such as Zn2+, Cu2+, and Sn2+.
WO2002086043 (Unilever, 2002) describes a detergent bar composition which improves water retention in the bar by incorporation in the bar of a layered inorganic hydrotalcite like material comprising one or more bipositive metal ion and a tripositive metal ion. The publication also describes the layered inorganic material being generated insitu by mixing the mixed metal oxide precursor with the soap mass in the presence of water.
In most of the above publications, hydrotalcite type materials or mixed metal oxides have been incorporated in topical leave-on compositions which essentially comprises a cation which has anti-microbial activity. In WO2002086043, a hydrotalcite type layered material was incorporated in a wash off formulation e.g. a detergent bar for cleaning fabrics or for personal wash use for improved water retentivity in the bar and therefore is not a leave-on product. US5154932 (Dow Corning, 1992) describes formulations or products which exhibit anti-bacterial activity by the addition thereto of an effective amount of at least one mixed metal hydroxide conforming substantially to the formula Lim DdT(OH)(m+2d+3+na) (An)a.xH20 where m is zero to one, D is a divalent metal, d is from 0 to 4, T is a trivalent metal, A is an anion or a negative valence radical, (M+2d+3+na) is equal to or greater than 3, (m+d) is greater than zero, and xH20 represents excess waters of hydration. A highly preferred compound according to this invention is MgAI(OH)5-y Cly . xH2O. Although this compound comprises cations that do not have antimicrobial property, the compound itself is reported to have anti-bacterial property. However there is no report of any deodourant benefits. Further, there is yet a need felt in the art for providing for a composition that gives improved malodour control when used on skin and does


not use anti-bacterial moities thereby minimizing any effect on the delicate balance of the microflora on the skin.
The present inventors have now incorporated mixed metal oxide comprising of one metal from group II which does not have any anti-microbial activity and one from group III, in a composition for topical application which surprisingly provides for synergistic improvement in malodour control.
OBJECTS OF THE INVENTION
It is thus an object of the present invention to provide for a composition for topical application that has improved malodour control.
It is another object of the present invention to provide for a composition for topical application that in addition to giving improved malodour control, does not disturb the delicate balance of the microflora present on the skin.
It is yet another object of the present invention to provide for a composition for topical application that in addition to giving improved malodour control without disturbing the delicate balance of the microflora present on the skin, utilizes ingredients that are easily available and safe to use on the skin thereby providing for a highly efficient, inexpensive and safe product that can be used by a large population.
SUMMARY OF THE INVENTION
According to the present invention there is provided an improved composition for topical application for deodourant benefit comprising
(a) 0.5 - 40% of a mixed metal oxide having the general formula
(M)a(N)bOc wherein M is a group II divalent cation not having antimicrobial property and N is a group III trivalent cation and a has a value in the range of 0.3 to 0.9, b has a value in the range of 0.1 to 0.3 and c = 1
(b) 10- 99.5% of a topically acceptable carrier.

It is particularly preferred that, the group II divalent cation is magnesium or
calcium and the group III trivalent cation is aluminum.
The topically acceptable carrier is preferably free of water.
DETAILED DESCRIPTION OF THE INVENTION
The essential feature of the invention is the incorporation of certain mixed metal oxides in compositions for topical applications that provides improved malodour control.
Mixed metal oxides
The mixed metal oxide is represented by the general formula
(M)a(N)bOc wherein M is a group II divalent cation not having antimicrobial property and N is a group III trivalent cation and a has a value in the range of 0.3 to 0.9, b has a value between 0.1 and 0.3 and c = 1. The divalent cation is preferably chosen from magnesium, manganese, iron, cobalt, nickel, or calcium. The trivalent cation is preferably chosen from aluminium, chromium, manganese, iron, cobalt, nickel or lanthanum. It is particularly preferred that, the . divalent cation is magnesium or calcium, more preferably magnesium and the trivalent cation is aluminium. The general formula of the mixed metal oxide represented above can be stoichiometric or non-stoichiometric. When the mixed metal oxide is stoichiometric, the conditionality 2a + 3b + (-2c) = 0 holds 'gbo'd: (The composition of the invention may comprise precursors of the mixed metal oxide in addition to the mixed metal oxides. These precursors may be layered double hydroxide or hydrotalcite precursor materials which have the general formula:
(M) (N)x (OH)y (A-0)z. fH2O where A is an interlayer anion like (C03)"2, (N03)"1 , (S04)"2, (P04)"3, or (B407)"2 where e refers to the valency of the interlayer anion, x has a value between 0 and 1, y has a value between 0.1 and 4 , z has a value between 0 and 1, and f has a value from 0 to 10 and wherein the charge neutrality is maintained by


having (2+3x) - (y + ez) = 0. It is also possible to have partial substitutions by other metal ions.
The mixed metal oxides are prepared from the precursor materials by heating it to high temperatures, a process known as calcination. The temperature of calcination is preferably in the range of 300 - 700 °C, more preferably in the range of 450-550 °C.
The layered double hydroxides or hydrotalcite like materials e.g. hydrotalcite carbonates are prepared by combining appropriate stoichiometric amounts of aqueous solutions of metal salts/co-mixtures of metal salts with aqueous sodium carbonate solutions at typically high temperatures of 80-90°C. The precipitate containing the layered inorganic material is filtered and washed thoroughly with copious amounts of water to remove all soluble electrolytes. This wet cake obtained is subjected to drying to bring the moisture levels down to less than about 40% to produce a free flowing powder. Examples of layered materials are hydromagnesite, hydrotalcites with carbonate, nitrate, sulphate, tetraborate as inter layer anions.
The present inventors have confirmed by experimentation that the mixed metal oxides of the invention are far superior in malodour efficacy as compared to the precursors like mixed metal hydroxides e.g. hydrotalcite carbonate. As an example it was determined that the kinetics of the interactioh between rr^xed magnesium aluminium oxide with isovaleric acid which is a deodourant compound is kinetically much faster and more efficient as compared to that with mixed magnesium aluminium hydroxide carbonate.
The mixed metal oxides suitable for use in the present in invention are typically white powders and preferably have an average particle size in the range 1 to 20 microns, more preferably in the range of 5 to 12 microns. In case the particle size is larger the material is subjected to milling to get the desired particle size


range. The mixed metal oxide used in the composition of the invention typically contains approximately 5 to 10% moisture and is free flowing in nature.
The mixed metal oxide is present in the composition of the invention at 0.5 to 40%, preferably from 0.5 to 30 % and more preferably from 1 to 20% by weight of the composition.
Without wishing to be bound by theory', it is believed that the mixed metal oxide of the invention or the precursors thereof interact synergistically with the topically acceptable carrier of the composition to provide for highly efficient absorption/adsorption of the malodour produced from the metabolic byproduct of the microflora on the skin without effecting.the natural growth of the microflora.
Topically acceptable carrier
The composition comprises 10 to 99.9%, preferably 10 to 80% of a topically acceptable carrier. The topically acceptable carrier is any substance in the powder, gel, stick or cream state which can be safely applied on to the skin. It is particularly preferred that the carrier has very small amount of water, if at all. If water is present, it is preferably present in an amount less than 20%, more preferably less than 10%, further more preferably less than 5%. Of the various states in which the composition may be present, it is preferred that the composition is in the stick form or the powder form.
By stick form is meant a coherent solid mass containing one or more deodorant active constituents. Conventionally sticks adopt the form of solid rods, which are usually housed within a barrel container, typically of circular or elliptical cross section, that is open at one end through which the stick can protrude. However, other shapes, such as tablets, cakes or bars can be contemplated alternatively and likewise other container shapes for the sticks.
The deodorant sticks are usually manufactured by extrusion, casting or injection moulding or any other technique known in the art.


The carrier that is incorporated in the stick compositions employed herein comprises one or more liquid materials that is fluid at dispensing temperatures for the composition and can be gelled or otherwise structured by the structurant to provide a semi or solid product at use temperature, i.e. typically below 40 and usually below 30° C. Where one or more of the remaining constituents is itself fluid at dispensing temperatures, such as a short chain mono or di hydric alcohol or polyol having a melting point of below 40° C, it can provide the carrier function as well and the presence of an additional carrier is optional. The carrier can be hydrophilic or hydrophobic or a mixture of both. In many embodiments, the carrier or a major fraction of the carrier is hydrophobic, generating an oil phase.
One class of carriers that has found particular favour in recent years, and which is particularly desirable in formulations in accordance with the present invention, comprises liquid siloxanes and particularly volatile polyorganosiloxanes, i.e. liquid materials having a measurable vapour pressure at ambient conditions. The polyorganosiloxanes can be linear or cyclic or mixtures thereof. Preferred cyclic siloxanes include polydimethylsiloxanes and particularly those containing from 3 to 9 silicon atoms and preferably not more than 7 silicon atoms and most preferably from 4 to 5 silicon atoms, otherwise often referred to as cyclomethicones. Preferred linear siloxanes include polydimethylsiloxanes containing from 3 to 9 silicon atoms. The volatile siloxanes normally by themselves exhibit viscosities of below 10 centistokes, and particularly above 0.1 centistokes, the linear siloxanes normally exhibiting a viscosity of below 5 centistokes. The volatile silicones can also comprise branched linear or cyclic siloxanes such as the aforementioned linear or cyclic siloxanes substituted by one or more pendant --O-Si (CH 3 ) 3 groups. Examples of commercially available silicone oils which are employable include Dow Corning 344, Dow Corning 345 and Dow Corning 244, Dow Corning 245 and Dow Corning 246, (from Dow Corning Corporation) Silicone 7207 and Silicone 7158 (from Union


Carbide Corporation) and SF1202 (from General Electric [US]). Volatile silicones are often present in a proportion ranging from 20 to 50%.
The carrier employed in compositions herein can alternatively or preferably additionally comprise non-volatile silicone oils, which include polyalkyl siloxanes, polyalkylaryl siloxanes. and polyethersiloxane copolymers. These can suitably be selected from dimethicone and dimethicone copolyols. Commercially available non- volatile silicone oils include Dow Corning 556 and Dow Corning 200 series.
Non-silicone organic carriers include liquid aliphatic hydrocarbons such as mineral oils or hydrogenated polyisobutene, often selected to exhibit a low viscosity. A further example of liquid hydrocarbons comprises polydecene. Mixtures of silicone and non-silicone carriers can suitably be employed herein. The carrier or mixture of carrier employed in the present invention can be and in many effective compositions is anhydrous, i.e. contain no free water.
The structurant or structurants that are included in compositions moulded by the processes described . herein can comprise inorganic thickeners or organic structurants. The choice of structurant normally takes into account the chemical nature of the fluid phase which is being converted to a solid.
Organic structurants employable herein can be non-polymeric or polymeric. Non-polymeric structurants, including waxes and gellants, are often selected from fatty acids or salts thereof, often containing from 12 to 30 carbons such as stearic acid or sodium stearate, and/or fatty alcohols (typically insoluble in water) often containing from 12 to 30 carbons such as stearyl alcohol. Other organic structurants can comprise waxes such as paraffin waxes, hydrogenated castor oil, Synchrowax® HRC, Carnabau, beeswax, modified beeswaxes, microcrystalline waxes, polyethylene waxes and fatty ester derivatives of polyols, such as glycerol monostearate and related compounds.


A further preferred form of the carrier is the powder form. A particularly preferred form of the powder carrier as per the invention is as a talcum powder. The powder carrier material is preferably chosen from talc, mica, mineral silicates and mixtures thereof.
Micas which may also be used in the present invention are in particular muscovite, phlogopite, tiotite, sericite, lepidolite, paragonite and artificial or synthetic mica having a fluorine atom substituted for the hydroxyl group of natural mica as well as baked or calcined products thereof. Such micas may be used alone or in any mixture thereof.
Mineral silicates useful in the present invention are for example phyllosilicates and tectosilicates such as pyrophylite, chlorite, antigorite, lizardite, kaolinite, dickite, nacrite, halloysite, montmorillonite, nontronite, saponite, sauconite, and bentonite; natrolites such as natrolite, mesolite, scolecite, and thomsonite; heulandites such as heulandite, stilbite, epistibite; and zeolites such as analcite, harmotone, phillipsite, chabazite and gmelinite. Such silicate minerals may be used alone or in combination. The phyllosilicates may have organic cations at the interface of the layers thereof or may be substituted with alkali metal or alkaline earth metal ions. The tectosilicates may include metallic ions in the fine pores thereof.
The most highly preferred carrier material is talc. Talc is a magnesium silicate mineral material, with a" sheet silicate structure and a composition of Mg3Si4(OH)22 and may be available in the hydrated form. It has a plate like morphology and is essentially oleophilic / hydrophobic i.e they are wetted by oil rather than water. Talc provides good lubricity or slip and has acceptable fragrance retention. Conventionally, talcum powder formulations can vary in complexity from merely talc and perfume to over a dozen components, especially in some products directed towards specific use.


The topically acceptable carrier is preferably present in an amount of 30 to 99%, more preferably from 60 to 99% by weight of the composition. Average particle size of topically acceptable carrier in powder form according to the present invention preferably ranges from 1 to 20 microns, more preferably from 5 to 12 microns.
Optional ingredients
Other optional ingredients such as fillers, colour, perfume, opacifier, preservatives, one or more water soluble/insoluble particulate materials such as alumina, borax, kaolin, polysaccharides, liquid benefit agents such as sunscreens, moisturisers, emollients, anti-ageing compounds, and other conventional ingredients may be incorporated in the composition.
The invention will now be Illustrated with the help of non-limiting examples of the compositions according to the present invention.
EXAMPLES 1 TO 4
Samples were prepared using isovaleric acid (IVA) as the model malodour compound. IVA solutions in water at specific concentrations were prepared. To 10 ml of this solution was added predetermined amounts of an inorganic powder as listed in Table-1.
The mixed metal oxide in this set of examples were prepared by .heating the precursor double layered hydroxide i.e. magnesium aluminium hydrotalcite with the formula Mg6Al2 (C03) (OH)16. 4 H20, to a temperature of 550 °C for one hour. An XRD pattern of the mixed metal oxide sample is shown as Figure-1.
The mix of the IVA solution and the inorganic powder was vortexed vigourously to ensure good mixing. The mix was equilibrated by incubation at 30 °C for 20 hours. The suspension was then centrifuged for 20 minutes at 8000 rpm and the supernatant solution was analysed by gas chromatography (GC) for IVA


content. The percentage reduction in IVA was calculated from the concentration thus determined and the initial IVA concentration.
Table-1

Example No IVA
concentration (ppm) Talc (mg) Mixed Magnesium Aluminium oxide (mg) Percentage reduction in IVA concentration
1 1000 100 74
2 1000 - 100 97
3 100 500 - 78
4 100 - 500 100
The data in table -1 indicates that the mixed metal oxide reduces the level of IVA far superior to talc.
EXAMPLES 5 TO 7
Further samples were prepared using the same procedure as examples 1 to 4 with the IVA solutions in water at 50 ppm as listed in table-2. The suspensions were then scored for malodour by an expert panel of three trained panelists on a scale of 1 to 5 where 1 denotes no smell and 5 denotes very strong smell. The malodour scores (as an average of three readings) are listed in Table- 2.
Table-2

Example No Talc (mg) Magnesium Aluminium oxide (mg) Malodour score
5. 500 - 1.00
6. - 50 0.65
7. 450 50 0.20
The data in table-2 indicates that a mix of talc and the mixed meal oxide provides for synergistic improvement in malodour reduction.

WE CLAIM:
1. A composition for topical application comprising:
(a) 0.5 - 40% of a mixed metal oxide having the general formula (M)a (N )bOc
wherein M is a divalent cation not having antimicrobial property chosen from magnesium, manganese, iron, cobalt, nickel, or calcium and N is a trivalent cation chosen from aluminium, chromium, manganese, iron, cobalt, nickel or lanthanum and a has a value in the range of 0.3 to 0.9, b has a value in the range of 0.1 to 0.3 and c =1
(b) 10- 99.5% of a topically acceptable carrier.
2. A composition as claimed in claim 1 wherein the divalent cation is magnesium.
3. A composition as claimed in claim 1 wherein the trivalent cation is aluminium.
4. A composition as claimed in claim 1 wherein the mixed metal oxide is prepared from precursor materials by heating the same to a temperature in the range of 450 to 550°C.
5. A composition as claimed in claims l wherein the mixed metal oxide is present in amount of 1 to 20% by weight of the composition.

6. A composition as claimed in any of the preceding claims wherein the water content is less than 5% by weight of the composition.
7. A composition as claimed in any of the preceding claims wherein the composition is in the powder or stick form.
8. A composition as claimed in any of the preceding claims wherein the topically acceptable carrier is talc.
Dated this 28th day of June 2005 Dr. Sanchita Ganguli
Of S. Majumdar & Co. Applicant's Agent


Documents:

698-mum-2004-abstract (complete).doc

698-mum-2004-abstract (complete).pdf

698-mum-2004-abstract(30-06-2004).doc

698-mum-2004-abstract(30-06-2004).pdf

698-mum-2004-claims (complete).doc

698-mum-2004-claims (complete).pdf

698-mum-2004-claims(granted)-(30-06-2004).doc

698-mum-2004-claims(granted)-(30-06-2004).pdf

698-mum-2004-correspondence(ipo)-(27-06-2008).pdf

698-mum-2004-correspondence-received-240506.pdf

698-mum-2004-correspondence-received-280605.pdf

698-mum-2004-correspondence-received.pdf

698-mum-2004-correspondence1(24-05-2006).pdf

698-mum-2004-correspondence2(14-02-2008).pdf

698-mum-2004-description (complete).pdf

698-mum-2004-description (provisional).pdf

698-mum-2004-drawing(30-06-2004).pdf

698-mum-2004-drawings.pdf

698-mum-2004-form 1(30-06-2004).pdf

698-mum-2004-form 13(03-10-2007).pdf

698-mum-2004-form 13(29-09-2008).pdf

698-mum-2004-form 18(24-05-2006).pdf

698-mum-2004-form 2(granted)-(30-06-2004).doc

698-mum-2004-form 2(granted)-(30-06-2004).pdf

698-mum-2004-form 3(28-06-2005).pdf

698-mum-2004-form 3(30-06-2004).pdf

698-mum-2004-form 5(28-06-2005).pdf

698-mum-2004-form-1.pdf

698-mum-2004-form-18.pdf

698-mum-2004-form-2 (complete).doc

698-mum-2004-form-2 (complete).pdf

698-mum-2004-form-2 (provisional).doc

698-mum-2004-form-2 (provisional).pdf

698-mum-2004-form-3-300604.pdf

698-mum-2004-form-3.pdf

698-mum-2004-form-5.pdf

698-mum-2004-power of attorney(14-11-2007).pdf

abstract1.jpg


Patent Number 224110
Indian Patent Application Number 698/MUM/2004
PG Journal Number 06/2009
Publication Date 06-Feb-2009
Grant Date 29-Sep-2008
Date of Filing 30-Jun-2004
Name of Patentee HINDUSTAN LEVER LIMITED
Applicant Address HINDUSTAN LEVER HOUSE, 165/166, BACKBAY RECLAMATION, MUMBAI 400 020, MAHARASHTRA, INDIA.
Inventors:
# Inventor's Name Inventor's Address
1 SHAH NIMISH HARSHADRAI 17 POSTAL COLONY, AZAD NAGAR, ANDHERI EAST, MUMBAI 400 099 MAHARASHTRA, INDIA.
2 PRAMANIK AMITAVA 64 MAIN ROAD, WHITEFIELD, BANGALORE 560 066, KARNATAKA, INDIA.
3 CHAKRABARY DEBOJIT F-12/12 HARINIKETAN CHS, BANGUR NAGAR, GOREGAON WEST, MUMBAI 400 090, MAHARASHTRA, INDIA.
PCT International Classification Number A 61 K 7/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA