(21) Application Number: KElP/ 2010/ 001199
(22) Filing Date: 23/06/2009
(30) Priority data: 1440/MUM/2008 10/07/2008 IN
(86) PCT data EP2009/057813 23/06/2009 wo 2010/003819 14/01/2010
(73) Owner: UNILEVER PLC ofUnilever House, 100 Victoria Embankment, London EC4Y ODY, United Kingdom
(72) Inventors: MANTHENA, Vamsi Krishna ofHindustan Unilever Research Centre, B.D. Sawant Marg Chakala, Andheri (East), Mumbai 400 099, India; PEDRO, Andre Messias Krell ofUnilever Brazil Ltda Av, Invernada 401, Valinhos CEP 13271-450 Sao Paulo, Brazil; STEVENS, Deborah ofUnilever R&D Port Sunligh, Quarry Road East, Bebington, Wirral Merseyside CH63 3JW, United Kingdom; HOPTROFF, Michael John ofUnilever.R&D Port Sunlight, Quarry Road East, Bebington, Wirral Merseyside CH6W, United Kingdom; LEOPOLDINO, Sergio Roberto ofUnilever Brazil Ltda, A v Invernada, 401, Valinhos CEP 13271-450 Sao Paulo, Brazil; PLUMMER, Christopher of7 James Avenue, Great Sutton, Ellesmere Port Cheshire CH66 4LP, United Kingdom; RAGHA VACHARl, Raj an ofHindustan Unilever Research Centre, B.D. Sawant Marg, Chakala, Andheri (East), Mumbai 400 099, India and TRIVELIN, Luciano Augusto ofUnilever Brazil Ltda, Av Invernada, 401, Valinhos, CEP 13271-450 Sao Paulo, Brazil.
(74) Agent/address for correspondence:, Kaplan & Stratton Advocates, P.O. Box 40111-00100, Nairobi
(54) Title: A PERSONAL WASH COMPOSITION
(57) Abstract: The present invention relates to personal wash compositions. The personal wash composition according to the invention comprises: (i) 10% to 55% Total Fatty Matter; and (ii) 0.1 wt% to 1.2 wt% chelating agent. The personal wash compositions according to the invention exhibit relatively high antibacterial activity.
A PERSONAL WASH COMPOSITION
The present invention relates to personal wash composit!ons.
5 The invention has been developed primarily for use in personal wash application and will be described hereinafter with reference to this application. However, it will be appreciated that the invention is not limited to this particular field of use.
10 Any discussion of the prior art throughout the specification should in no way be considered as an admission that such prior art is widely known or forms part of the common general knowledge in the field.
Personal wash compositions are available in various forms such as bars, liquid
15 soaps, creams and gels. Commercial soap compositions often have one or more "soaps", which means "salts of carboxylic fatty acids". The counter-ions of the salts are generally sodium, potassium, ammonium or alkanolammonium ions, but other suitable ions known in the art are also used, though their use is
relatively uncommon. Compositions based on soap bars generally contain from
20 40% to about 76% total fatty matter, more popularly known in the art in its abbreviated form "TFM". According to Indian IE?gislation, soaps having TFM in
the range of 60% to 76% are called "Toilet soaps" and are classified into grades I, II and Ill depending on the TFM content. On the other hand, soap bars with TFM in the range of40% to 60% are commonly known in the art as "Bathing
25 bars". The analytical methods for determining the TFM level of soaps are well known in the art. ~tructuring agents and fillers are generally included in such compositions.
_Several bacteria prefer to live and multiply on the human skin. Some of these 30 bacteria are known to cause body odour, pimples and acne. There is some
evidence in the prior art to suggest that some of these conditions aggravate in a hot and humid climate. It is known that soaps, i.e. salts of fatty acids, per-se, have antimicrobial properties.
5 The increasing demand for vegetable oils, such as palm oil, (one of the main sources of oils and fatty acids used by soap manufacturers), and consequent soaring prices has led to severe constraints on the sustainability of the soaps and detergents Industry, as it is becoming increasingly difficult to provide high TFM soaps at a competitive cost, while still making reasonable profits.
As a result, the trend is towards lower TFM soaps, being a cod-effective measure. However, lowering of TFM has a direct and negative effect on the• antimicrobial or antibacterial property of the soap compositions. In order to restore the antimicrobial activity, actives such as Triclosan (i.e. 2,4,4'-trichloro-
15 2'-hydroxy-diphenylether;TCN), Triclocarbanilide (TCC), Benzalkonium• chloride or other widely recognised antimicrobial agents are gener91ly added to personal wash compositions. However, the long-term, continued use of both TCN and TCC has come under the scanner of environmentalists•and consumer
bodies due to concerns over bio-degradation. It is therefore desirable to stop
20 using these agents, or at least minimise their use.
Soap bars with relatively lower TFM have been described in prior art.
A low TFM soap bar has been described in W02006/094586 (HINDUSTAN
25 LEVER LTD). The composition includes 15% to 30% TFM, 25% to 70% inorganic particulates including talc and calcium carbonate, 0.5% to 10% • aluminosilicate; and 3% to 20% water. There is no reference to the antibacterial activity of the resultant compositions.
GB2319181 (RECKITT & COLMANN PRODUCTS LTO, 1999) states that the activity of many antimicrobial agents may be improved by the use of chelating agents, and such agents are often used in antiseptic soaps, It is said that . chelating agents are often used as stabilizing agents in the soap base but are
5 frequently added again during manufacture of the finished soap, in the belief that they will increase antimicrobial activity. The patent discloses antiseptic soap bar which includes 0.35 to•0.75 wt% of chlorinated methyl substituted
phenol (an antimicrobial), 0.15 to 0.25 wt% Triclosan (or a salt thereof); and less than 0.075 wt% EDTA as the chelating agent. It is said that there are a
10 number of drawbacks associated with the use of chelating agents, notably their co.st; their potential as irritants and their environmental impact, and for these re9sons, the levels of chelating agents has been kept to a minimum.
GB1169551 (Unilever, 1970) describes super-fatted detergent bars containing
15 as preservative a synergistic mixture of at least 0.005 wt% ethane-1- hydroxy-1, 1-diphosphonic acid (EHDP) and 0.005 wt% ethylenediamine tetra acetic acid (EDTA) by weight of the bar. The EHDP, the EDTA or both may be in the form of their esters or salts. It is said that by incorporating the above mixture of
sequestering agel!ts in C3 detergent bar, a bar is obtained which is especially
20 resistant to the development of rancidity, spotting or overall ,discoloration. There is no reference to the antibacterial/antimicrobial.efficacy of the resultant bars.
It may be seen from the above-mentioned related art that addition of
antibacterial agents to boost the antibacterial/antimicrobial activity, has been the
25 method of choice.
There still is an unmet need for antibacterial personal wash compositions having relatively lower TFM and relatively lower antibacterial agents.
It is an object of the present invention to overcome or ameliorate at least one of the disadvantages of the prior art.
A further object of the present invention is to provide personal wash
5 compositions having relatively lower TFI\!1, which exhibit relatively high antibacterial activity.
It is another object of the invention to provide a personal wash composition which is particularly effective against gram negative bacteria.
It is another object of the present invention to provide a personal wash composition which not only exhibits significant bacteriostatic action (Le. inhibition of bacterial growth), but also significant bactericidal action (i.e. the ability to kill bacteria)
"other objects of the present invention will become apparent to those skilled in the art by reference to the specification.
The present inventors have surprisingly found that personal wash compositions
20 comprising TFI\!1 in the range of 10% to 55% and 0.1 wt% to 1.2 wt% chelating agent exhibit relatively high degree of bacteriostatic and bactericidal activity.
According to the first aspect, the present invention provides a personal wash composition comprising:
25 (i) 10% to 55% total fatty matter; and
(ii) 0.1 wt% to 1.2 wt% chelating agent.
Preferred chelating agent is a salt of ethylenediamine tetra acetic acid or a salt of diethylene triamine penta acetic acid.
Preferably the TFM is from 30% to 50%, and more preferably from 40% to 50%.
According to the second aspect, the present invention pr.ovides use of a personal wash composition according to the first aspect for antibacterial benefit.
According to the third aspect, the present invention provides a method of cleansing skin comprising the step of contacting the skin with a personal wash composition according to the first aspect.
10 The term "comprising" is meant not to be limiting to any subsequently stated elements but rather to encompass non-specified elements of major or minor functional importance. In other words the listed steps, elements or options need
not be exhaustive. Whenever the words "including" or "having" are used, these
. terms are meant to be equivalent to "comprising" as defined above.
Except in the operating and comparative examples, or where otherwise explicitly indicated, all numbers in this description indicating amounts of material ought to be understood as modified by the word "about".
20 It should be noted that in specifying any range of concentration or amount, any particular upper concentration can be as$ociated with any particular lower concentration or amount.
For a more complete understanding of the above and other features and
25 advantages of the invention, reference should be made to the following detailed description of preferred embodiments.
The term Total Fatty Matter, abbreviated to "TFM", is used to denote the
percentage by weight of fatty acid and triglyceride residues present in the
30 personal wash composition without taking into account the accompanying
cations. For a soap having 18 carbon atoms, an accompanying sodium cation will generally amount to about 8% by weight. Other cations may be employed as desired, for example zinc, potassium, magnesium, alkyl ammonium and aluminium. To calculate the "soap" level in the personal wash composition, the
5 TFM level is to be multiplied by 1.08.
Personal wash compositions may be in a solid form or a non-solid form.
Personal wash compositions in solid form are particularly preferred. The total •fatty matter is 10% to 55% by weight of the personal wash composition. When
10 the personal wash composition is in solid form, the total fatty matter is preferably 25 to 55%, more preferably 30% to 50%, and most preferably 40% to
50%. When the personal wash composition is in a non-solid form; the-total fatty matter is preferably from 10 to less than 25%, more preferably from 1•2 to 20%. It has been observed by the present inventors that lowering of antimicrobial
1-5 performance as assessed by Minimum Inhibitory Concentration (MIC) and the Minimum Bactericidal Concentration (MBC) test is significant when the total fatty matter (TFM) content in personal wash composition is reduced from 50% to 30%, as against reducing TFM content from 70% to 50%. The predominant wash-active agent in the detergent composition of the present invention is
20 conventional soap, otherwise referred to as fatty acid salt. The soap may be derived from one or a mixture of Cs-Czz, preferably C1z-C1s straight or branched chain, saturated or unsaturated monocarboxylic acids of natural or synthetic origin. Natural sources e.g. animal, marine or vegetable fats and oils, almost always yield mixtures of these fatty acids, all of which may be employed.
25 Examples thereof include the fatty acids derived from coconut oil, olive oil, palm kernel oil, tall oil, soy bean oil, cottonseed oil, peanut oil, safflower oil, sunflower seed oil, corn oil, fish oils and tallow. Illustratively, individual fatty acids include capric, lauric, myristic, stearic, oleic, palmitic, palmitoleic, ricinoleic, linoleic, and
linolenic acid. The fatty acids may also be derived synthetically by paraffin
30 oxidation and oxo-synthesis. The cation or salt portion of the soap is preferably
an alkali metal, su~h as potassium and, especially sodium, but may alternativ.ely be an alkaline earth metal.
A preferred soap is a mixture of about 30% to about 40% coco"nut oil and about
5 60% to about 70% tallow. Mixtures may also contain higher amounts of tallow, for example, 0.01% to 20% coconut and remaining tallow. The soaps may contain unsaturation in accordance with commercially acceptable ~tandards. Excess.ive unsatur.ation is preferably avoided.
10 It is essential that the personal wash compositions of the present invention include 0.1 vvt% to 1.2 wt% chelating agent. Preferred chelating agents are as follows (names followed by their abbreviation in parenthesis):
EthyleneDiamine Tetra Acetic acid (EDTA), Diethylene Triamine Penta Acetic
15 acid (DTPA), Ethane-1-hydroxy-1, 1-diphosphonate (EHDP), EthyleneDiamine-N,N'-Disuccinate(EDDS),. Nitrile Triacetic Acid (NTA), Sodium Imino Disuccinate (IDS), Ethylene Glycol-bis-(2-aminoethyi)-N,N,N',N'-TetraAcetic
acid (EGTA), Methyl Glycine Diacetic Acid (MGDA), N-(2-hydroxyethyl) EthyleneDiamine N,N',N'-Triaceticacid) (HEDTA), EthyleneDiamine Tetra
20 Methylene Phosphonic acid (EDTMP), Diethylene Triamine-Penta-Methylene Phosphonic acid (DTPMP), Glutamic acid-N,N-Diacetic Acid
(GLDA), Cyclohexane-1 ,2-Diamine-N,N,N',N'-Tetra-AceticAcid (CDTA), 1,3-Propylenediamine Tetra-Acetic Acid (PDTA), EthyleneDiamine Triacetic Acid (EDTA), L-hydroxy Imino Disuccinic acid (L-IDS), Trisodium N-Carboxyethyl
25 Imino Succinate (CEIS), Citric Acid, Sodium Tripolyphosphate (STP), Triethylene Tetramine Hexaacetic Acid (TTHA). Other.preferred chelating agents are Trisodium EthyleneDiamine Disuccinate, Tetra-sodium-Imino disuccinate, Glutamic acid-N,N diacetic acid tetra sodium salt, 2-hydroxyethyl
iminodiacetic acid, Sodium salt (disodium ethanol diglycinate), Tetrasodium 3-
30 hydroxy-2,2 imino disuccinate, Trisodium methylglycine diacetic acid, L-
Aspartate-N,N-diacetic acid tetrasodium salt. The more preferred chelating agents are salt of EthyleneDiamine Tetra Acetic acid (EDTA) and salt of Diethylene Triamine Penta Acetic acid (DTPA). Preferre.d salts of EDTA are disodium Ethylene Diamine Tetra Acetic acid and tetrasodium EthyleneDiamine
5 Tetra Acetic acid. Preferred salt ofOTPA is the pentasodium Diethylene Triamine Penta Acetic acid.
The salt form is preferred over acid form, as addition of the chelating agents in the acid form would bring about a corresponding decrease in pH, which is not
10 desirable. It is preferred that the salt of Ethylene Diamine Tetra Acetic acid or Diethylene Triamine Penta Acetic acid is present from 0.1 wt% to 0.4 wt%. It is-further pre•ferred that the composition includes a combination of 0.1 wt% to 0.4
wt% salt of EthyleneDiamine Tetra Acetic acid and 0.1 wt% to 0.4 wt% salt of
Diethylene Triamine Penta Acetic acid. At significantly low TFM (i.e.TFM from
15 25% to 55%), the present inventors have observed that salt of EDTA exhibits two optima, at respectively 0.1 wt% and 0.4 wt% for significantly superior performance in terms of bacteriostatic and bactericidal activity, whereas
increasing salt of DTPA was observed to continuously increase the antibacterial
performance. Of the two, salt of DTPA shows better antibacterial performance.
20 The salt of DTPA exhibited optima at 0.3 wt% and 0.4 wt% in the personal wash composition. With 50% TFM in soap, salt of DTPA showed better efficacy at 0.2 wt% level than salt of EDTA. However with 30% TFM in the composition; salt of OTPA has been found to be better than salt of EDTA even at 0.1 wt% level.
25 The technical benefit of this invention is in improving the antibacterial benefits while lowering the TFM content of the personal wash composition. It has been observed by the present inventors that by increasing chelating agents in the personal wash composition, especially in bar form, the antibacterial
performance against E. coli, a typical gram negative bacterium, is significantly
30 improved. Transient gram negative bacteria are the cause of diseases and
hence irY)proving performance of the personal wash composition against them, by increasing chelating agent level in the personal wash compositi.ons offers significant benefits to the consumers.
5 Gram-negative bacteria are those bacteria, which do not retain crystal violet dye in the Gram staini~g protocol. Gram-positive bacteria, on the other hand retain the crystal violet dye when wash.ed in a decolorizing solution. In a Gram stain
test, a counter-stain (com.monly Safran in) is added after the crystal violet, colouring all Gram-negative bacteria red or pink. The test itself is useful in
1 0 classifying two distinct types of bacteria based on structural differences in their cell walls. Of these two classes of organisms, Gram negative bacteria are the dort}inant cause ,of serious public health diseases such as diarrhoea. It is well known in the prior art that the incidence of diseases such as diarrhoe? may be r~duced byefiective skin cleansing using soap based products.
It has been observed by the present inventors that when acidic filler such as starch is added to the. personal wash composition, it reduces the pH of the comp.osition. It has been further observed by the present inventors that the preferred pH of thE? c?mposition is from 9 to 11 .5, and more preferably from 9.8
20 to 10.8. This can be achieved by addition of an alkali such as sodium hydroxide or sodium carbonate, more preferably sodium carbonate. The preferred level of
alkali is from 0.1 wt% to 1.0 wt%, more preferred being 0.25 wt% to 0.5 wt%. The pH of the composition is measured at 30 oc at a concentration of 10 wt%.
25 In addition to th.e ingredients described above, the compositions ofthe present invention preferably. include a filler so as to fill the formulation space, arising out of the lower TFM of the composition. A highly preferred filler is starch. Suitable starch materials include natural starch (from corn, wheat, rice, potato, tapioca and the like), pre-gelatinzed starch, various physically and chemically modified
30 starch and mixtures thereof. By the term natural starch is meant starch which
has not been subjected to chemical or physical modification; also known as raw or native starch.
A preferred starch is natural or native starch from maize (corn), cassava, wheat,
5 potato, rice and other natural sources of it. Raw starch with different ratio of amylose and amylopectin: e.g. maize (25% amylose); waxy maize (0%); high amylose maize (70%); potato (23%); rice (16%); sago (27%); cassava (18%); wheat (30%) and others. The raw starch can be used directly or can be
modified during the process of making the bar composition such that the starch
10 becomes gelatinized_, either partially or fully gelatinized.
Another suitable starch is pre-gelatinized which is starch that has been
gelatinized before it is added as an ingredient in the present bar compositions.
Various forms are available that will gel at different temperatures, e.g., cold
15 water dispersible starch. One suitable commercial pre-gelatinized starch is supplied by National Starch Co. (Brazil) under the trade name. FARfv1AL TM CS 3400 but other commercially available materials having similar characteristics are suitable.
20 The amount of starch can preferably range from about 5 wt% to 25 wt%, more preferably 6 wt% to 25 wt%, further more preferably 10 wt% to 25 wt%, and most preferably 10 wt% to 15 wt% of the composition.
When it was attempted by the present inventors to fill-in the formulation space
25 with a filler, e.g. starch (due to the lower TFM), it was observed that the pH of the composition dropped significantly, and so did the antibacterial activity. Merely increasing the pH of the composition did not produce any appreciable results.
In addition to TFM and chelating agent, the composition preferably also includes an anionic surfactant at 0.05 wt% to 10 wt%, more preferably 0.5 wt% to 8 wt%, and most preferably 1 wt% to 5 wt%. It has been observed by the present inventors that addition of synthetic surfactant e.g. sodium Iaury! sulphate (SLS)
5. boo;:;ts the antimicrobial benefit. Especially suitable surfactants are water soluble salts of organic sulphuric reaction products having in the molecular structure an alkyl radical containing from 8 to 22 carbon atoms., and a radical
chosen from .sulphoniG acid or sulphur acid ester radicals and mixtures thereof. Preferred anionic surfactants include sodium Iaury! sulphate, alpha olefin
10 sui phonates, sodium Iaury! ether sulphate and primary alcohol sulphates .
. The other non-soap surfactants such as nonionic, cationic, and zwitterionic, or amphot~ric surfactants Gan also be used for added benefits e.g. for mildness or to boost lather.
Suitable.nonionic: su~actqnts can be broadly described as compounds produced by the condensation of alkylene oxide groups, which are hydrophilic in nature, with an organic hydrophobic compound which may be aliphatic or alkyl aromatic in nature. The length of the hydrophilic or polyoxyalkylene radical
20. which is condensed. with any particular hydrophobic group can be readily ;adjwsted t? yi~ld. a water-soluble compound having the desired degree of balance between hydrophilic and hydrophobic elements.
Suitable amphoteric surfactants that optionally can be employed are derivatives
25 of aliphatic secondary and tertiary amines containing an alkyl group of 8 to 18 carbon atoms and an aliphatic radical substituted by an anionic water-solubilizing group, for instance sodium 3-dodecylamino-propionate, sodium 3-dodecylaminopropane sulphonate and sodium N-2-hydroxydodecyi-N-
Suitable cationic surfactants are quaternary ammonium salts having an aliphatic
radical of from 8 to 18 carbon atoms, for instance cetyl trim ethyl ammonium
5 Suitable zwitterionic surfactants that can be employed are derivatives of aliphatic quaternary ammonium, sulphonium and phosphonium compounds having an aliphatic radical of from 8 to 18 carbon atoms and an aliphatic radical
substituted by an anionic water-solubilising group, for instance 3-(N-N-dimethyi-
N-hexadecylammonium), propane-1-sulphonate betaine, 3-(dodecylmethyl
10 sulphonium) propane-1-sulphonate betaine and 3-(cetylmethylphosphonium) ethane sulphonate betaine.
Further examples of suitable surfactants are compounds commonly used as
surface-active agents given in the well-known textbooks "Surface Active
15 Agents", Volume I by Schwartz and Perry and "Surface Active Agents and Detergents", Volume II by Schwartz, Perry and Berch. The surfactants under this invention are compounds other than soap whose detersive properties, like soap, are due to the presence of a hydrophilic and a hydrophobic group in the molecule.
In addition to the above essential ingredients, the personal wash compositions of the present invention may also comprise any or all of the following ingredients used to increase the shelf life, aesthetics or functionality, namely:
25 -Vitamins such as vitamin A and E, and vitamin alkyl esters such as vitamin C alkyl esters; lipids such as cholesterol, cholesterol esters, lanolin, ceramides, sucrose esters, and pseudo-ceramides; liposome forming materials such as phospholipids, and suitable amphiphilic molecules having two long hydrocarbon chains; essential fatty acids, poly unsaturated fatty acids, and sources of these
30 materials; triglycerides of unsaturated fatty acids such as sunflower oil, primrose
oil, avocado oil, almond oil; vegetable butters formed from mixtures of saturated and !Jnsaturated fatty acids such as shea butter; mineral such as sources of zinc, magnesium, and iron; skin conditioners such as silic<?ne oils, gums and modifications thereof sucl1 as linear and cyclic polydimethylsiloxanes, amino,
5 alkyl, and alkylaryl silicone oils; hydrocarbons such as liquid paraffins, petrolatum, Vaseline ™, microcrystalline wax, ceresin, squalene, pristan, paraffin wax a~d mineral oil; conditioning proteins such as milk proteins, silk proteins and glutins; cationic polymers as conditioners which may be used include QUATRISOFT™ LM-200 POLYQUATERNIUMTM_24, MERQUAT™
10 Plus 3330, POLYQUATERMIUM™ 39; and JAGUAR™ type conditi<~>ners, humectants suGh as glycerol, sorbitol, and urea; and emollients such as esters of long chain fatty_ acids, such as isopropyl palmitate and cetyl lactate.
F,urth~r, the composition •can be made multicoloured, e.g., striped, through the :15 judicious use of. dye as is well known in the art.
. Finally, perso~al wash Gompositions, when in solid form, generally comprise about 1 wt% to 30.wt%, preferably 2 wt% to 25 wt%, more preferably 3 wt%-to 1.6 wt% water. The amount of water may be significantly higher, up to 90%
20 when the personal WC!Sh compositions are in non-solid form.
It is highly preferred that the personal wash compositions of the present invention are in ''bar"form.
25 The soap bars of the invention are preferably prepared by milling and plodding, the melt cast process may also be used. The process may be carried out in any mixer conventionally used in soap manufacture, and is preferably carried out in a high shear-kneading mixe~. The preferred mixers include ploughshare mixer, mixers with kneading members of Sigma type, multi-wiping overlap, single
30 curve or double arm. The double arm kneading mixers can be of overlapping or
the tangential design. Alternatively, the invention can be carried out in a helical screw agitator vessel, or multi-head dosing pump/high shear mixer and spray drier combinations, as in conventional process.
5 The invention will now be •described in greater detail with reference to the following non-limiting examples.
10 Formulations of the personal wash compositions
Various personal wash compositions (in soap.:.bar form) were made and tested for their antibacterial efficacy. The basic formulations of the compositions used in the examples which follow, are given in Table 1 below:
70% TFM 64% TFM 54% TFM 48% TFM 30% TFM
(A) (B) (C) (D) (E)
Sodium soap of fatty acid * 75.6 69.1 58.3 51.8 32.4
Corn starch 0 0 14 14 25
Talc 8 6 5 5 5
Sorbitol (100%) 1 6 6 6 10
Sodium Iaury! sulphate (SLS) 0 2.5 4 4 4.0
Alpha olefin sulfonate (AOS) 0 0 0 0 0
Trichlorocarbanilide 0.2 0.1 0.1 0.1 0.1
Fragrance, color, preservatives 2 2 2 2 2
and other minors
Water to 100% to 100% to 100% to 100% to 100%
*This number is obtained by multiplying the% TFM by a factor of 1.08.
In experimental bars, wherever a salt of EDTA or salt of DTPA, and/or sodium carbonate was incorporated in the compositions; the same has been indicated in the relevant example; and an equivalent amount of water was reduced from
5 the ~omposition., to keep the sum total of all ingredients in th.e composition at 100%. The bars were prepared using conventional equipment used in the manufacture of extruded soap. In summary, the bar was prepared by combining soap noodles with the remaining ingredients in Table 1 in a Z-blade
mixer and passing the mixture through a 3-roll mill and a refiner. The soap
10 noodles were composed of a mixture of lauric-rich and stearic-rich soaps used in a weig~t ratio inthe range from 40/60 to 10/90. The lauric-rich soaps were
. derived from palm kernel oil, coconut oil and/or babasu oil. The stearic-rich soaps were derived from tallow, palm oil, palm stearine, hardened soybean oil and crude soybean oil. The compositions so processed were added to the
15. hopper of a two stage ext~uder and extruded at a temperature of 35°C at an extrusion rate of1 .2 - 4.0 kg/minute through an eye plate having a 3.5 x 3.5 em cross section to form billets cut to about 12 em in lengths. The billets were then transferred to a manual soap stamper and stamped to form the finished
personal 'Nashcomposition in bar form utilizing a die set defining a mould
20 having a volume of approximately 79 to 80 cm3 (density in the range from 1.12
. to 1.14 g/cm3).
25 The following two analytical methods were used to determine the bacterial kill and bacterial growth inhibition of various compositions.
Bacterial kill assay
All the experiments on this assay were conducted against E. coli and as such represent a model of performance against Gram-negative pathogens
5 responsible for diseases such as diarrhoea.
An aqueous (1 0 wt %) slurry of the personal wash composition (in bar form) is prepared. At time zero, the bacterial suspension is added to this slurry. Addition
of this bacterial suspension decreases the product concentration from 'I0% to
10 8% (which is a typical in use concentration for soap bars). The test slurries are stirred and after a specified contact time (typically between 30 seconds and 5 minutes) a sample is recovered and transferred to a quenching solution to stop any further antimicrobial activity. The sample is then diluted and placed onto a suitable growth media, such as Tryptone Soy Broth (bacterial growth media)
15 and incubated at a suitable temperature (typically between 28°C and 37 oC). The number of colonies is counted after 18-24 hours of incubation. From this number, the number of bacteria killed whilst in .contact with the test slurry is calculated and expressed in terms of log reduction in bacterial numbers. Higher log reduction indicates higher antimicrobial activity in terms of baderial kill.
Bacterial growth inhibition assay
An aqueous (1 0 wt %) slurry of the personal wash composition (in bar form) is prepared. The test slurry is repeatedly diluted in bacterial growth media such
25 as Tryptone Soy Broth. A standard bacterial inoculum of E. coli is then added to each dilution of test slurry and the samples are incubated as above. In this way, a series of samples is generated, with varying concentration of the formulation.
An effective composition would show appreciable inhibition of growth of bacteria
at a comparatively lower concentration than the reference material. The
30 percentage of replicates displaying growth at each dilution was counted to
provide an indication of how dilute the product may be while still delivering an antibacterial effect in terms of inhibition of bacterial growth. The more potently antibacterial a product is, the more dilute it may be whilst still inhibiting bacterial growth.
Effect of TFM on bacterial kill and inhibition of bacterial growth
10 In this experiment, the effect of varying TFM on bacterial kill and inhibition in the growth of bacteria (E. coli) was studied. 10% slurries o•f each of the Compositions A, D and E (as in Table 1 above) were used for this experiment and the bacterial kill•and inhibition was determined by the respective methods given above. All the compositions were devoid of any chelating agent.
30 48 70
(Composition E) (Composition D) (Composition A)
Log 1.25 2.5 3.7
-%samples 90 62 45
20 Table 2 shows the effect of TFM on bacterial kill (E. coli) at a contact time of 5 minutes, in terms of log reduction in the number of bacteria. Table 2 also shows
the percentage of samples displaying growth. Higher growth indicates lesser efficacy.
The results indicate that the ability of the personal wash composition to kill and
5 to inhibit growth of E. coli is directly proportional to the TFM. Example 2
Effect of chelating aoent on bacterial kill
In this example, the bacterial kill provide by personal wash compositions according to the invention (at 54% and 48% TFM, compositions C and D of Table 1 respectively, with 0.15 wt% pentasodium DTPA) was compared against
. a commercial 70% TFM soap (composition A of Table 1 devoid of chelating
15 agent) and a comparative 64% TFM soap containing antibacterial active (composition B of Table1 devoid of chelating agent). The kill was determined at a contact time of 2 minutes and 5 minutes for all the compositions by the methodology described above.
%TFM 48% 54% 64% 70%
Composition- D Composition- C Composition Composition-A
of table-1 with - B of table-1 of table-1
of table-1 with 0.15
0.15wt% wt% Pentasodium No chelating No chelating
Pentasodium salt salt of DTPA agent agent
minutes minutes minutes minutes
2 5 2 5 2 5 2 5
Log reduction 4.0 5.3 4.3 6.5 5.1 8.2 3.9 6.9
5 The. results in the above table indicate appreciable log reduction in bacterial numbers (which is a marker of bacterial kill) at relatively lower TFM of 48% and 54%, in the presence of 0.15 wt% pentasodium DTPA.
Effect of che!ating agent on inhibition of bacterial growth
In this experiment, the inhibition of bacterial growth of 48% and 30% TFM compositions containing varying levels of disodium EDTA and pentasodium
15 DTPA (compositions C and D ofT able 1 respectively, containing varying levels of chelating agents) was compared against a commercial 70% TFM soap (composition A of table-1, devoid of chelating agent). The bacterial inhibition was determined by the method given above. Results of this experiment are
presented in Table 4 below.
%TFM % chelating Percentage of
48% 0.1 40
(Composition D of Table 1
containing disodium salt of EDTA)
(Composition D of Table 1
containing Pentasodium salt of DTPA)
30% 0.3 15
(Composition E of Table1 containing
pentasodium salt of DTPA)
70% 0 47
Composition A of Table 1
5 The results in Table 4 indicate that the addition of pentasodium DTPA or disodium EPTA to a 48% TFM soap composition leads to relatively higher inhibition of bacterial growth, when compared to a 70% TFM commercial soap devoid of chelating agent. Similar results can be seen upon inclusion of pentasodium DTPA in 30% TFM soap.
Effect of chelating agent and pH on bacterial kill
5 I~ this experiment, the effect of chelating agent and pH on bacterial kill was studied on a 48% TFM soap bar (composition D of Table 1) containing 0.15 wt% pentasodium salt of DTPA and varying levels of Na2C03, to vary the pH of• the compositions. An equivalent amount of water was reduced from the compositions to compensate for the added ingredients. The kill was determined
10 at a contact time of 2 minutes and 5 minutes for all the compositions, by the methodology described above. The data on bacterial kill is presented in Table 5
below. The Table also includes comparative results obtained with commercial 70% TFM bars devo~d of chela~ing agent (composition A of Table 1 devoid of chelating agent), as well as a .64% TFM soap devoid of chelating agent
15 (composition B of Table 1 devoid of chelating agent). The pH of the compositions was measured at 10% aqueous solution concentration at 30°C .
%TFM . wt% chelating agent, and wt% pH Log reduction
2 minutes 5 minutes
48 0.1.5; 0.2 10.2 5.4 8.2
48 0.:15; 0.5 10.8 6.2 7.0
48 0.15; .1.0 11.5 7.5 8.0
64 0;0 10.62 5.0 8.2
70 0;0 10.45 4.0 7.0
The data indicates that increasing pH further improved the antibacterial effect of the chelating agent at 48% and 54% TFM soap compositions with chelating agents.
5 Example 5
Effect of varving levels of chelating agent and pH on bacterial kill
In another set of experiments, the effect of van;ing levels of chelating agent and
10 pH, while keeping the TFM constant was studied. In these experiments, a series of 48% TFM soap compositions (composition D of Table 1) were prepared, which contained varying leveis of chelating agent (pentasodium DTPA) and sodium carbonate (to vary the pH). An equivalent amount of water was reduced
from the compositions to compensate for the added ingredients. These
15 compositions were tested for bacterial kill in a 2 minute contact time experiment by the method described above. The results of these experiments are presented in Table 6 below. For comparison, the results were compared against 70% TFM and 64% TFM soap compositions, devoid of chelat.ing agent or sodium carbonate (compositions A and B of Table 1 respectively).
%TFM Pentasodium DTPA /%wt NazC03 Ievel/wt% pH Log reduction
48% 0.1 0.1
0.15 0.1 10.45 7.1
0.2 0.1 10.39 7.1
. '0.1 0.2 10.65 7.1
0.15 0.2 10.65 /.1
0.2 0.2 10.64 7.1
0.1 0.25 10.77 7.0
0.15 0.25 10.82 7.0
0.2 0.25 10.83 7.0
0.1 0.5 10.75 7.0
0.15 0.5 10.81 7.0
0.2 0.5 10.83 7.0
0.1 1.0 10.91 7.0
0.15 1.0 10.88 7.0
0.2 1.0 10.92 7.0
70% - 10.45 5.8
64% - 10.62 6.4
The above resUits•indicate that a combination of pH and chelating agent gives
5 comparatively higher log reduction, even at a short contact time of 2-minwtes.
Effect of combination of chelating agents
5 In yet another set of experiments, the effect of a combination of chelating agents on the bacterial kill (log reduction at 2 minute contact time) was studied for the compositions having the formulation as given in Table 7 below.
Ingredients(%) Composition . H---~- I
Sodium Soap 52 52 52
Corn Starch 14.00 14.00 14.00
ifalc ~.00 5.00 5.00
Sorbitol (1 00%) 6.00 6.00 p.OO
Titanium Dioxide 0.40 0.40 0.40
Disodium EDT A 0.04 0.04 0.04
EHDP 0.02 0.02 0.02• -
Pentasodium DTPA 0.20 0.20 0.10
Sodium Carbonate 0.00 0.25 0.10
Sodium Laury! Sulphate 2.00 ~.00 2.00
Alpha Olefin Sulphonate 2.00 2.00 2.00
Moisture 16.00 16.00 16.00
Fragrance, color and other minors ifo 100 ifo 100 To 100
The TFM of all compositions was 48%, and the soap bars were prepared by the method used to prepare soap bars of compositions in Table 1. The bacterial kill efficacy of above compositions was tested as per methodology given above,
and. the re$ults obtained are presented in Table 8 below. The results have been compared with that of 64% TFM and 70% TFM soap compositions of Table 1.
Composition Log reduction pH
A (of Table 1) 4.9 10.45
B (of Table 1) 6.9 10.62
F 6.5 10.57
G 7.0 10.65
H 6.2 10.62
Thus, it can be readily seen that combinations-of chelating agents also provide comparatively higher log reduction.
It will be appreciated that the illustrated examples, provide for personal wash. ••10 compositions having relatively low TFM having relatively high degree of
antibacterial activity. It will also be appreciated that the illustrated examples provide personal wash compositions which are particularly effective against Gram negative bacteria E. coli. It will also be appreciated that the illustrated examples provide personal wash compositions which not only exhibit significant
15 bacteriostatic action (i.e. inhibition of bacterial growth), but also significant bactericidal action (i.e. the ability to kill'bacteria)
It should be understood that the specific forms of the invention herein illustrated
and described are intended to be representative only as certain changes may
20 be made therein without departing from the clear teachings of the disclosure.
Although the invention has been described with reference to specific embodiments, it will be appreciated by those skilled in the art that the invention may be embodied in many other forms.
1. A personal wash composition comprising:
(i) 10% to 55% Total Fatty Matter; and
5 (ii) 0.1 wt% to 1.2 wt% chelating agent.
2. A personal wash composition as claimed in claim 1 wherein the chelating agent is a salt of ethylenediamine tetra acetic acid or a salt of diethylene triamine penta acetic acid.
3. A personal wash composition as claimed in claim 2 INherein the salt of ethylenediamine tetra acetic acid or said salt of diethylene tria mine penta acetic acid is from 0.1 wt% to 0.4 wt%.
15 4. A personal wash composition as claimed in claim 2 or claim 3 wherein said salt of ethylene diamine tetra acetic acid is disodium ethylene diamine tetra acetic acid salt or a tetrasodium ethylenediamine tetra acetic acid.
5. A personal wash composition as claimed in claim 2 or claim 3 wherein said
20 salt of diethylene triamine penta acetic acid is a pentasodium diethylene triamine penta acetic acid.
6. A personal wash composition as claimed in any one of the preceding claims comprising 5 wt% to 25 wt% starch.
7. A personal wash composition as claimed in any one of the preceding claims wherein the Total Fatty Matter is 25% to 50% when the personal wash composition is in solid form.
8. A personal wash composition as claimed in any one of the preceding claims 1-6 wherein the Total Fatty Matter is 10% to less than 25% when the personal wash composition is in non-solid form.
5 9. A personal wash composition as claimed in any one of the preceding claims wherein pH of the composition is from 9 to 11.5.
10. A personal wash composition as claimed in claim 9 wherein the pH of the composition is from 9.8 to 10.8.
11. A personal wash composition as claimed in any one of the preceding claims comprising 0.05 wt% to 10 wt% anionic surfactant.
12. A personal wash composition as claimed in claim 11 wherein the anionic
15 surfactant is selected from sodium lauryl sulphate, alpha olefin
sui phonates, sodium lauryl ether sulphate or primary alcohol sulphates.
13. Use of a personal wash composition 9S claimed in claim 1 for antibacterial benefit.
14. A method of cleansing skin comprising the step of contacting the skin with a personal wash composition according to any one of claims 1 to 12.
(21) Application Number: KElP/ 2010/ 001199