Cold processable non-toxic preservative composition for home and personal care products

Abstract

Disclosed herein is a cold-processable antimicrobial composition in non-dusting solid form, free from toxic antimicrobial comprising, a) N-capryloyl glycine (Formula I), b) N-undecylenoyl glycine (Formula II), c) benzoic acid (Formula III) and d) sodium dehydroacetate (Formula IV) for use in personal care and home care products. The invention further discloses a process for preparation of the antimicrobial composition and ease of its incorporation in various personal and home products.

Claims

1. A cold-processable antimicrobial composition in non-dusting composite blend form, comprising a) N-capryloyl glycine, b) N-undecylenoyl glycine, c) benzoic acid, and d) sodium dehydroacetate; wherein a. benzoic acid and sodium dehydroacetate are used in a 1:1 ratio by weight; and b. the cold-processable antimicrobial composition does not include phenoxyethanol.

2. The cold-processable antimicrobial composition of claim 1, wherein the cold-processable antimicrobial composition is free of surfactants.

3. A process for preparation of a cold-processable homogeneous antimicrobial composition in non-dusting composite blend form which is free of surfactants, comprising N-capryloyl glycine, N-undecylenoyl glycine, benzoic acid, and sodium dehydroacetate in a ratio of 1:1:1:1 by weight, comprising: a) Melting a blend of N- Capryloyl glycine and N-undecylenoyl glycine in 1:1 ratio by weight to obtain molten mass; b) Adding benzoic acid and sodium dehydroacetate in 1:1 ratio by weight to the molten mass under stirring at about 75 C. till the reaction mass becomes clear; and c) Cooling the blend to obtain preservative composition in the form of non-dusting composite blend.

4. The process according to claim 3, wherein the non-dusting solid form may be selected from the group consisting of cubes, flakes, granules, powder, a compact, and combinations thereof.

5. A personal care composition comprising the antimicrobial composition of claim 1 in an amount of 0.3 to 2% of the personal care composition.

6. The personal care composition according to claim 5, wherein the personal care composition is selected from the group consisting of a powder, granules, a compact, a lotion, a cream, a solution, a body-washes, sera, a hand wash, an intimate hygiene wash, a wipe, an emulsion, and combinations thereof.

7. A home care composition comprising the antimicrobial composition of claim 1 in an amount of 0.3 to 2% of the home care composition.

8. The home care composition according to claim 7, wherein the home care composition is selected from the group consisting of a powder, granules, a lotion, a cream, a solution, a wipe, an emulsion, a dish washing formulation, a surface cleanser, and combinations thereof.

9. The cold-processable antimicrobial composition of claim 1, wherein N-capryloyl glycine, N-undecylenoyl glycine, benzoic acid, and sodium dehydroacetate are used in a 1:1:1:1 ratio by weight.

Description

DESCRIPTION OF DRAWINGS

(1) FIG. 1 shows 1a) typical flake form of the composition 1b) aqueous fine dispersion at 1% at room temperature and 1c) depicts clear solution of this dispersed antimicrobials at room temperature in the presence of 8 to 10% surfactant mix, typically anionic or amphoteric surfactants.

(2) FIG. 2 shows particle size analysis of the aqueous dispersion showed that d(0.5) is 97 and d(0.9) is 214.

DETAILED DESCRIPTION OF INVENTION

(3) The present invention relates to a broad spectrum, cold processable antimicrobial preservative composition in the form of non-dusting composite blend for use in personal care and home care products.

(4) The term blend, as used in the specification refers to an admixture of 1) N-capryloyl glycine (CG), 2) N-undecylenoyl glycine (UG), 3) benzoic acid (BA) and 4) sodium dehydroacetate (SDA).

(5) The phrase composite blend as used in the specification refers to the composition obtained as per the process described in example 2.

(6) As described in the background, most of the highly efficient preservatives of yesteryear are seriously mired into toxicity issues and are being consciously phased out by the personal care industry. These include parabens, isothiazolinones, formaldehyde releasers, chlorinated molecules, brominated molecules, iodinated substances, phenolic molecules and quaternary ammonium type molecules. Some manufacturers of antimicrobial preservatives (Table I in the background of the invention section) came up with idea of blending safe antimicrobials like organic acids with phenoxyethanol. However, in view of certain reservations about phenoxyethanol for the want of adequate safety data and its structural similarity with toxic glycol ethers, a need is felt by the present inventors to create antimicrobial compositions without phenoxyethanol. Phenoxyethanol is a CNS depressant and the reasons for requesting reassessment and the restrictions imposed are explained in the background section. Hence there remains a definite need for antimicrobial preservative compositions for personal and home care products without phenoxyethanol. This need has been partly addressed by replacing phenoxyethanol by benzyl alcohol. Only a couple of compositions are in the market wherein phenoxyethanol has been replaced by benzyl alcohol. The compositions have been created using benzyl alcohol along with other organic acids. Benzyl alcohol has strong benzaldehyde like odor and that restricts its usage in personal care formulations. Even today, phenoxyethanol is more widely used than benzyl alcohol. (October 2016, Mintel, where Ingredient Search matches one or more of [Phenoxyethanol, Benzyl Alcohol] as the Ingredients; Mintel Group Ltd is a privately owned, London-based market research firm.) Thus, it can be seen by referring to Table 1 in background section that benzyl alcohol is not a good substitute for phenoxyethnol since several antimicrobial blends in the market today are based on phenoxyethanol.

(7) Accordingly, in an embodiment, the present patent invention provides efficacious preservative composition in the form of non-dusting composite blend which comprises well-known and well accepted personal care ingredients. The composition of the present invention is based on four organic acids that address the safety and efficacy problems adequately by providing the coverage against both bacteria and fungi. The preservative composition of the present invention comprises a combination of 1) N-capryloyl glycine (CG), 2) N-undecylenoyl glycine (UG), 3) benzoic acid (BA) and 4) sodium dehydroacetate (SDA), wherein, the ratio of the N-capryloyl glycine:N-undecylenoyl glycine:benzoic acid:sodium dehydroacetate may range from 1:1:1:1.

(8) Details of the Components of the Present Composition

(9) Lipoaminoacids (N-acylated amino acids) are described in WO 92/20647, WO 92/21318, WO 94/26694, and WO 94/27561 as amphiphilic biological vectors that are advantageous as regulators of skin physiology and are shown to be suitable for many different applications in cosmetics.

(10) N-Capryloyl Glycine:

(11) ##STR00003##

(12) N-capryloyl glycine, also known as N-octanoyl glycine (CAS No. 14246-53-8) is also well-known for its action against naturally occurring micro-flora that is resident of skin. The use of this antimicrobial was suggested way back in 1996, as a non-preservative substance that can inhibit microbial growth in cosmetics (Proserpio, Gianni; Cattaneo, Roberta C & T, Edizione Italia 17(3), 11-13, 16-19, (1996). It offers derma-protection for the restoration of the skin's acid mantle and purification through dandruff reduction by the inhibition of Pityrosporum ovale. It is commercially available under the trade name Lipacide C8G from SEPPIC.

(13) N-Undecylenoyl Glycine:

(14) ##STR00004##

(15) Almost four decades ago N-undecylenoyl amino acids were reported for the treatment of skin disorders (JP 49093521, 1974). One of them is N-Undecylenoyl glycine (CAS No 54301-26-7) is a well-known derma-purifier with very pronounced anti-acne and anti-dandruff activity. It is commercially available under the trade name Lipacide UG from SEPPIC, France. SEPPIC reported (FR 2771632 A1) cosmetic compositions containing undecylenoyl glycine along with capryloyl glycine in 1999. Corinne Stolz, (US 20010002257A1) disclosed compositions comprising undecylenoyl glycine and capryloyl glycine along with tannin rich plant extracts that showed activity against skin flora. Interestingly, in 2004, use of combination of Wasabi extract along with undecylenoyl glycine and capryloyl glycine as co-preservatives for protection of personal care preparations was reported by D. Misner (U.S. 2004/096528 A1). Kabara et al. (U.S. Pat 2007/0196315 A1) reported preserved botanical extracts with capryloyl glycine, undecylenoyl glycine, glyceryl monolaurate and pentylene glycol.

(16) Benzoic Acid:

(17) ##STR00005##

(18) Maximum allowed concentration of benzoic acid (CAS No 65-85-0) (Cosmetics Directive Annex VI) is 2.5% in rinse-off and 0.5% in leave-on product. For oral products the permissible concentration is 1.7%. It is well-known antimicrobial with specific action against fungi. Hence it is widely used in food products as preservative.

(19) Sodium Dehydroacetate:

(20) ##STR00006##

(21) Maximum authorized concentration of sodium dehydroacetate (CAS number 520-45-6) according to Cosmetics Directive Annex VI is 0.6%. In the USA and EU the maximum allowed concentration is 0.6% whereas in Japan is it is 0.5% in the final personal care products. It is a good fungicide and mild bactericide.

(22) In another preferred embodiment, the invention provides process for preparation of preservative composition in the form of non-dusting composite blend which comprises; a) Melting a blend of N-capryloyl glycine and N-undecylenoyl glycine in 1:1 ratio by weight to obtain molten mass; b) Adding benzoic acid and sodium dehydroacetate in 1:1 ratio by weight to the molten mass under stirring at about 75 C. till the reaction mass becomes clear; and c) Cooling the blend to obtain non-dusting solid form of preservative composition.

(23) The cooled composite blend can be obtained in the non-dusting solid forms such as cubes, flakes (example 2), granules etc. by pouring the same in shaped molds or by spreading it on a metal or glass surface uniformly or by spray drying to obtain in granules etc.

(24) According to this process a blend of N-Capryloyl glycine and N-undecylenoyl glycine (1:1 by weight) is synthesized in one pot as described in Example No 1. The dry powder of mixture of N-capryloyl glycine and N-undecylenoyl glycine in (1:1 ratio by weight) is then melted (90 C.) under nitrogen atmosphere and to this stirred molten mass, benzoic acid and sodium dehydroacetate (1:1 ratio by weight) are added and stirring is continued at 75 C. till the reaction mass becomes clear. This molten composite blend is then flaked by spreading it on a metal or glass surface uniformly to get a very thin (2 to 4 mm) off-white flakes upon cooling and scraping (Example 2). The melting point range of these flakes is from 55 to 65 C. and acid value ranges from 235 to 240.

(25) The preservative composite blend in flake form thus obtained is completely free from dust explosion hazard and other health hazard to human while handling the material. The thin flake form avoids handling of these solid organic acids in powder form and the dust explosion hazard. The minimum ignition energy of 1:1 mixture of N-capryloyl glycine and N-undecylenoyl glycine is as low as 55 mJ. Using this process (Example 1 & 2) it is very apparent to anyone with reasonable knowledge in microbiology that ratios of four components can be varied a little and still can get the effective broad spectrum of antimicrobial activity, for example, ratio of N-capryloyl glycine:N-undecylenoyl glycine:benzoic acid:sodium dehydroacetate can be 1:1:1.25:0.75 or it can be 1.25:0.75:1.0:1.0 by weight. Many such combinations can be worked out with overall broad range of antimicrobial activity. However, excellent cold-processability results from the composition comprising N-capryloyl glycine:N-undecylenoyl glycine:benzoic acid:sodium dehydroacetate in the ratio of 1:1:1:1 by weight.

(26) In another embodiment, the present invention provides the advantage of cold-processability of the composite blend of the preservative composition.

(27) In addition to free of dust explosion hazard, ease of incorporation is the additional biggest advantage of the present invention. Typically, incorporation of solid antimicrobial is always a problem if it does not dissolve in water readily or in some other personal care ingredients. The incorporation of antimicrobial blend of the present invention in personal and home care formulations is extremely facile due to its low melting point (around 60 C.) which makes it easy to incorporate if the personal care formulation involves mixing of ingredients at elevated temperatures. The composite blend of the present invention is soluble in glycolic or alcoholic personal care ingredients such as propylene glycol, 2-ethylhexylglycerin, caprylyl glycol etc. Some of these liquid personal ingredients can be used to pre-dissolve the antimicrobial blend of this composition and then introduced to the rest of the formulation that is being stirred at room temperature or at elevated temperature. The properties of being low melting and of being soluble in common personal care ingredients offer a lot of ease-of-incorporation while formulating variety of personal care formulations. If the processing of the personal care or home care formulation does not involve heating at all then the blend of Example 2 is simply incorporated by a) stirring it with part of water for few minutes to form aqueous dispersion and b) adding all other ingredients (including surfactants) of the home care/personal care composition to this fine dispersion of antimicrobial blend and mixing is continued at room temperature to get the homogeneous mass (FIGS. 1a, 1b & 1c)).

(28) FIG. 1a shows the typical flake form of the composition of the present invention prepared in accordance with example 2, whereas FIG. 1b shows the aqueous fine dispersion of 1% at room temperature and FIG. 1c depicts clear solution of this dispersed antimicrobials at room temperature in the presence of 8 to 12% surfactant mix, typically anionic or amphoteric surfactants. This 8 to 12% surfactant mix is the usual range that can be used for home and personal care products. This ease of dispersion of the anti-microbial blend of the present invention in water and subsequent solubility of the same in the presence of surfactants is very surprising. The particle size analysis of the aqueous dispersion showed that d(0.5) is 97 and d(0.9) is 214 (FIG. 2). This aqueous suspension behavior is explained by the experiments enlisted in Table II.

(29) The data given in Table II is generated on 300 g scale experiments by dispersing 1% of antimicrobial preservative compositions in water & solubilizing the dispersed particles in the mixture of 10% sodium laureth sulphate and 2% cocamidopropyl betaine at the 300 rpm. The addition of individual ingredients (N-capryloyl glycine (CG), N-undecylenoyl glycine (UG), benzoic acid (BA) and sodium dehydroacetate (SDA) in 1:1:1:1 ratio by weight) to stirred water so as to get about 1% concentration at room temperature does not result in a dispersion (Table II, entry 1). Similarly, it should also be noted that the blend of four acids, namely, N-capryloyl glycine, N-undecylenoyl glycine, benzoic acid and dehydroacetic acid (DA) in the ratio of 1:1:1:1 by weight, does not get dispersed in water at any temperature (Table II, entry 2). In both cases upon addition of surfactants (sodium laureth sulphate 10% and cocamido propyl betaine 2%) and continued stirring of 3 h is needed for complete dissolution of the blend. However, the composite blend of the present invention in its flake form gets dispersed in water and its further dissolution in surfactant solutions at room temperature is very facile (1 h) (Table II, entry 4). It requires only .sup.rd of the time to dissolve in surfactant solution compared to the blend of all four-acids (entry 2).

(30) It is pertinent to mention here that the blend of N-capryloyl glycine, N-undecylenoyl glycine, dehydroacetic acid and sodium benzoate is inhomogeneous and does not show facile dispersion in water or dissolution in surfactants (Table II, entry 3), when compared to the composite blend of the present invention (Table II, entry 4). Also, it has been found that the blend of the present invention requires the entire quantity of dehydroacetic acid in its sodium salt for facile dispersion in water. Partial use of sodium salt of dehydroacetic acid along with partial amount of dehydroacetic acid (Table II, entry 5) results in losing the degree of ease of dispersion that is normally exhibited by the blend of present invention.

(31) Needless to say that with the facility of high speed, high shear mixing (Silverson type or any other rotor-stator type; http://www.silverson.com/us/products/laboratorymixers/) the dispersion time in water as well as solution time in the presence of surfactants are further reduced.

(32) But the order of relative ease of dispersion remains the same. For example, 1% dispersion (4 g of composition of Example 2 in 400 mL water) and dissolution (in the presence of 10% surfactants) with Silverson L5M-A mixer with Square hole high shear screen (at 3000 rpm and 25 C.) is accomplished in three minutes whereas the individual ingredients took about 10 min for creation of homogeneous dispersion and finally solution on the same scale. However, most of the industry uses cold process (without any heating) and simple mixing (and not high shear homogenizer) for personal care formulations like shampoos or hand-dish washes where batch size is usually 10 to 50 MT. It is uneconomical to heat such huge reaction mass and hence ease of cold dispersibility of solid ingredients does matter a lot in these industries.

(33) TABLE-US-00002 TABLE II Time taken for dissolution of 1% anti- microbial Time taken blend in for water in the dispersion of presence of 1% anti- surfactants microbial (300 rpm) 10% The composition blend in SLES and of anti-microbial Melting water 2% CAPB, blend Acid value point (300 rpm, rt.) at rt. 1 All four Does not 3 h ingredient in disperse isolated form UG, CG, BA and SDA 2 All four in acid 315 52-60 C. Does not 3 h form (1:1:1:1) as disperse one blend 3 UG/CG/DA Does not and sodium form a benzoate (1:1:1:1) homogeneous blend 4 UG/CG/BA and 240 55-65 C. Complete Complete SDA (1:1:1:1) dispersion in dissolution in (Example 2) 3 h 1 h 5 UG/CG/BA and 292 58-68 C. Does not 3 h SDA (1:1:1.5:0.5) disperse

(34) Cold processability of the preservative composition of the present invention is illustrated in Example 6. The pre-dispersed blend of Example 2 in water, is readily dissolved by anionic surfactants as demonstrated in Examples 5, 6 & 7. Example 5 illustrates cold processing of a hand dish wash that is preserved with antimicrobial composition of Example 2. In this example the dispersion of antimicrobial composition in water is made first and to this dispersion the other ingredients like lauryl ether sulphate, alkyl amine oxide and alkyl polyglucoside are added at room temperature. Example 6 illustrates the shampoo formulation effected at room temperature. To the dispersion of antimicrobial of the present invention in water, other ingredients like anionic surfactant and the amphoteric surfactant are added at room temperature. To this Galaxy Sparkle 660 (a pearlizer consisting of an alkanol amide and the pearly wax, Ethylene glycol distearate) is added and the whole is mixed at room temperature to get pearly shampoo. Such cold pearlizer compositions are available from several other manufactures like BASF (Euperlan), Lubrizol (QuickPearl) and Solvay (Mirasheen). In case of emulsion type formulation (Example 7), to an aqueous dispersion of the antimicrobials of the present invention, surfactants or other oily ingredients are added at room temperature and the whole mass is homogenized using Silverson type homogenizer till a uniform product is obtained. Thus, the preservative blend of the present invention exhibits equal ease of incorporation in aqueous surfactant based formulations (shampoo/shower gels type) as well as emulsion type cream formulations. Pre-dispersion of the anti-microbial composition of this patent application in water allows its incorporation to both rinse-off or leave-on type of formulations at room temperature.

(35) In another embodiment, the invention demonstrates antimicrobial efficacy of the antimicrobial blend of the present invention.

(36) The minimum inhibitory concentration (MIC) against bacteria, yeast and mold is given in Table III. It is to be noted that MIC numbers for the present antibacterial composite blend against all organisms is less than 0.5%. (Table III)

(37) The Minimum Inhibitory Concentration of Composition of Example 2 (Table III)

(38) TABLE-US-00003 TABLE III Microorganism MIC of Example 2 (% active) Staphylococcus aureus ATCC 6538 0.4 Pseudomonas aeruginosa ATCC 15442 0.4 Escherichia coli ATCC 8739 0.4 Candida albicans ATCC 10231 0.3 Aspergillus niger ATCC 16404 0.4 Propiniobacterium acnes MTCC 1951 0.3 Malassezia furfur MTCC 1374 0.3

(39) The preservation efficacy of composition of Example 2 was tested by incorporating it in two types of personal care formulations that have significant quantity of water, namely, a shampoo (rinse-off application, Example 3) and an oil-in-water cream formulation (leave-on application, Example 4) at about 1.0% active level. Both formulations were then challenged by inoculating various microbes as per the standard protocol of CTFA (Evaluation of preservatives to protect cosmetics by D. Orth in Cosmetics and Toiletries, March 91). The initial inoculation level of microbes for this study was around 10.sup.6 to 10.sup.7 cfu/ml for bacteria and 10.sup.5 for yeast and mold in the formulation. Both rinse-off and leave-on formulations passed the challenge tests and the results are tabulated in Tables IV and Table V. Aqueous formulations like shampoo with pH of 6.0 can be easily preserved with 0.5 to 0.75% of composition of the present invention. Similarly, emulsion type formulations can be preserved with 0.5% level of antimicrobial composition of the present invention. The antimicrobial composition of the present invention can be used for any personal care or home care formulation with or without significant amount of water in it. Examples of personal care formulation without water would be face powder or face wash. The solid nature of this present invention makes it amenable to solid personal care and home care products that are either free flowing powders or compact solids. Example 8 illustrates the solid composition of effervescent powder face cleanser.

(40) TABLE-US-00004 TABLE IV Challenge test as per PCPC: Shampoo (pH 6.0) with 1.0% composition of Example 2 48 7 14 21 28 Test Organisms 0 h Hours Days Days days Days Staphylococcus aureus 3.8 10.sup.6 <10 <10 <10 <10 <10 Escherichia coli 5.8 10.sup.6 <10 <10 <10 <10 <10 Propionibacterium acnes 4.0 10.sup.6 <10 <10 <10 <10 <10 Pseudomonas aeruginosa 2.8 10.sup.6 <10 <10 <10 <10 <10 Candida albicans 3.8 10.sup.6 <10 <10 <10 <10 <10 Aspergillus niger 5.7 10.sup.6 <10 <10 <10 <10 <10 Malassezia furfur 5.6 10.sup.6 <10 <10 <10 <10 <10

(41) TABLE-US-00005 TABLE V Challenge test as per CTFA: Cream (emulsion) at pH 6.0 with 1.0% composition of Example 2 48 7 14 21 28 Test Organisms 0 hr Hours Days days days Days Staphylococcus aureus 5.6 10.sup.6 <10 <10 <10 <10 <10 Escherichia coli 3.3 10.sup.6 <10 <10 <10 <10 <10 Propionibacterium 5.6 10.sup.6 5.2 10.sup.2 <10 <10 <10 <10 acnes Pseudomonas 1.3 10.sup.6 2.2 10.sup.1 <10 <10 <10 <10 aeruginosa Candida albicans 4.9 10.sup.6 <10 <10 <10 <10 <10 Aspergillus niger 8.2 10.sup.6 <10 <10 <10 <10 <10 Malassezia furfur 9.8 10.sup.6 <10 <10 <10 <10 <10

EXAMPLES

(42) The present invention is now described by way of working and non limiting illustrative examples. The details of the invention provided in the following examples is given by the way of illustration only and should not be construed to limit the scope of the present invention.

(43) Benzoic acid and sodium dehydroacetate were purchased from Ganesh Benzoplast, India and FenChem Group, China respectively. Caprylic acid and undecylenic acid were purchased form VVF Ltd, Mumbai, India. Milcoside was procured from LG, S. Korea. Rest of the ingredients were supplied by Galaxy Surfactants Ltd, India.

Example 1: Synthesis of Blend of N-Undecylenoyl Glycine and N-Capryloyl Glycine (1:1 by Weight)

(44) To a stirred mixture of glycine (225 g, 3.0 gmol) in water (1700 g) at 25 C. under nitrogen, was added mixture of capryloyl chloride (255 g, 1.54 gmol) and undecylenoyl chloride (255 g, 1.24 gmol) and sodium hydroxide solution (478 g of 48.5% aqueous solution, 5.8 mmol) simultaneously while maintaining temperature between 20 to 25 C. and pH between 9.5 to 10.5. The addition takes 4 to 5 hours depending on the efficiency of temperature control. The reaction mass was stirred for additional two hours. It was further acidified by addition of concentrated hydrochloric acid. The precipitated solid was filtered and washed with plenty of water to remove the mineral acidity. The mixture of lipidated glycines was obtained as solid powder (595 g, 95%) after vacuum drying at 65 C. The dried powder had moisture less than 1% and acid value of 258. The HPLC analysis of powder indicated it to nearly 50:50 ratio of N-undecylenoyl glycine and N-capryloyl glycine. The mixture of two lipidated glycines melts at 85 to 90 C.

Example 2: Preparation of Flakes of Composite Blend of N-Undecylenoyl Glycine, N-Capryloyl Glycine, Benzoic Acid and Sodium Dehydroacetate in the Ratio of 1:1:1:1 by Weight

(45) A mixture of N-undecylenoyl glycine, N-capryloyl glycine (500 g) from Example 1, under nitrogen was heated to 85-90 C. To the molten transparent mass, benzoic acid (250 g) and sodium dehydroacetate (250 g) were added and continued to stir for half an hour till the reaction mass became transparent. The reaction mass was converted into flakes by pouring over a cooled surface ensuring the thickness of flakes is 2 to 4 mm. The analysis of the flakes of the above composition is given in table below.

(46) TABLE-US-00006 Appearance/Nature Off-white Flakes Odour Characteristic pH (1% aqueous dispersion) 3.5 Acid Value, mg KOH/g 240 Moisture Content, % by mass <1% Melting point (in C.) 55-65

Example 3: Preparation of Shampoo and its Preservation with the Composite Blend of Example 2

(47) TABLE-US-00007 Components Trade Name (% W/W) Phase A Water (Aqua) DM Water 70.00 Sodium laureth sulphate (70%, 2 EO) Galaxy LES 70 20.00 Phase B Cocomonoethanol amide Galaxy 100 3.00 Ethylene glycol distearate Galaxy 610 2.00 Phase C Preservative Composition of 1.0 Example 2 Caustic Lye, 48% q.s. to pH 6 to 6.5 Fragrance, Color q.s

(48) Procedure:

(49) All the ingredients of phase A were heated to 75 C. under slow stirring. To this stirred Phase A, Phase B was added and mixed until homogeneous. The reaction mix was then cooled down to room temperature and phase C was added, and stirred until uniform consistency. pH of the final formulation was adjusted with 48% Caustic Lye and the fragrance and color were added and blended together.

Example 4: Preparation O/W Cream and its Preservation with the Composite Blend of Example 2

(50) TABLE-US-00008 Components Trade Name (% W/W) Phase A Water (Aqua) DM Water 70.00 Glycerin Glycerin 2.00 Phase B Paraffinum Liquidum Mineral oil 15.00 Stearic Acid Stearic Acid 2.00 Glyceryl Stearate Glyceryl Stearate 5.00 Cetearyl Alcohol Cetearyl Alcohol 3.50 Phase C Preservative Composition of Example 2 0.80 Fragrance, Color q.s

(51) Procedure:

(52) Heated the contents of Phase A and Phase B separately up to 75 C. with stirring. Added phase B to phase A with constant stirring. Homogenized for 2 minutes, continued stirring for 15 minutes. Added phase C. Mixed well Cooled the mass while mixing. Added fragrance and color when the mix is at room temperature and blended.

Example 5: Cold Process for Hand Dish-Wash and its Preservation with the Composite Blend of Example 2

(53) TABLE-US-00009 Components Trade Name (% W/W) Phase A Water (Aqua) DM Water 47.0 Sodium laureth sulphate (70%, 2 EO) Galaxy LES 70 21.5 Lauryl Amine Oxide, (30%) Galaxy LAO 6.0 Lauryl Glucoside (50%) Milcoside 200 4.0 Disodium EDTA 0.3 Phase B Sodium Chloride 1.0 Citric Acid 0.2 Preservative Composition of Ex 2 1.0 Water 20.0 Fragrance, Color q.s

(54) Procedure:

(55) Composition of Example 2 in Phase B was charged to the reactor with mentioned amount of water in Phase B and stirred for 15 min to get a fine dispersion of it. To this Phase A ingredients were added in the sequence and stirred at room temperature till a homogeneous mass is obtained (2 h). Sodium Chloride was added to the above mass and mixed. To this reaction mixture, color and fragrance were added to get the hand-dish wash. pH of the final formulation was adjusted to 5.5 with 50% citric acid.

Example 6: Cold Process for Shampoo and its Preservation with the Composite Blend of Example 2

(56) TABLE-US-00010 Components Trade Name (% W/W) Phase A Sodium laureth sulphate (70%, 2 EO) Galaxy LES 70 10.0 Cocoamidopropyl betaine Galaxy CAPB 2.0 Phase B Sodium Laureth Sulfate, Ethylene Galaxy Sparkle 10.0 glycol Distearate Cocamide MEA 660 Phase C Preservative Composition of 1.0 Example 2 Water (Aqua) DM Water 67.0

(57) Procedure:

(58) Phase C was charged to the reactor and stirred for 15 min to get a fine dispersion of preservative blend of Example 2. To this stirred Phase C, ingredients of Phase A were added sequentially and stirring was continued at room temperature. To the stirred mass cold pearlizer mix of Phase B was added and stirring was continued till a homogeneous mass is obtained (2 h). To this reaction mixture, color and fragrance were added to get the final shampoo. The pH of the final formulation was 6.0

Example 7: Cold Process of a O/W Cream and its Preservation with the Composite Blend of Example 2

(59) TABLE-US-00011 Components Trade Name (% W/W) Phase A Isopropyl Palmitate 9.5 Olive Oil 1.0 Vitamin E 0.1 Ethylhexyl methoxycinnamate Galaxy OMC (HP) 0.5 Phase B Hydroxyethyl cellulose Natrosol 250 1.0 HHR Glycerin 5.0 Laureth-7 Galaxy MW 257 5.0 Water 86.9 Preservative Composition of 1.0 Example 2 Phase C Caustic Lye, 48% 0.2 Fragrance q.s

(60) Procedure:

(61) Composition of Example 2 was dispersed in water under stirring for 15 min. Hydroxyethyl cellulose was added to the above dispersion slowly under stirring so that it swells uniformly in water. The remaining ingredients of Phase B were added to the above mass sequentially and mixed. Phase A ingredients were separately charge in another vessel and mixed at RT to form a homogeneous blend. Blend prepared with phase A ingredients was then added to Phase B mixture and homogenized for 5 min until a emulsion is obtained. Fragrance was added to the cream and pH of cream was adjusted to 6.0 with 48% caustic lye solution.

Example 8: Preservation of Effervescent Powder Face Wash with the Composite Blend of Example 2

(62) TABLE-US-00012 Components Trade Name (% W/W) Phase A Sodium Bicarbonate 33.8 Fumed Silica AEROSIL R-972 1.0 Phase B Citric Acid 25.2 Preservative Composition of 1.0 Ex 2 Sodium Lauryl Sulfate Galaxy LES (P) 19 Phase C Sodium Lauroyl Sarcosinate Galsoft NaLS (P) 20 Fragrance q.s

(63) Procedure:

(64) Ingredients of Phase A were mixed and then ingredients of Part B were added to Part A sequentially and mixed well. Part C ingredients were then added to above mixture and mixed well. The dry powder mixer was further pulverized to remove any gritty feel of powder. The pH of 5% solution of above formulation was 6.0.

Advantages of the Invention

(65) 1) The preservative composition of the present patent application avoids all toxic antimicrobials like parabens, halogenated chemicals, phenolic and alcoholic chemicals and formaldehyde releasers. The preservative composition of the present patent application is based on two lipidated glycines, namely, N-capryloyl glycine and N-undecylenoyl glycine and two organic acids, namely, benzoic acid and dehydroacetic acid in its sodium salt form. All ingredients are well accepted by the personal care industry, with proven benefits. All four ingredients of this composition are non-toxic to human. No adverse toxicity findings are reported in the literature so far.

(66) 2) The preservative composition of this patent application protects the personal care formulations from bacteria as well as from fungi. The combination of four antimicrobials with distinctly different structural features (straight chain aliphatic, cyclic aliphatic, aromatic, conjugated unsaturation, isolated unsaturation) would result in different mechanisms of attacking microbes that come with a variety of structural differences in the cell envelopes (glycocalyx, outer membrane and cytoplasmic membrane of non-nucleated Gram-ve and Gram-ve bacteria and nucleated fungi). Four pronged combinatory attack on a variety of microbes offered by the composition of the patent application lowers the dosage of individual ingredient significantly. The four pronged combinatory attack would also prevent the microbes from acquiring the resistance towards preservative composition. Use of several antimicrobials for preservation is a well-established defense strategy for restricting microbes from adapting and mutating to resistant forms.

(67) 3) The solid flake form of preservative composition of this patent application avoids any health hazard that might arise due to dusting of fine powder. The flake form also avoids the dust explosion fire hazard that is associated with fine dust of materials with lower MIEs (Minimum Ignition Energy). The composition can also be made in any other solid forms such as granules, cubes etc.

(68) 4) The preservative composition of the present invention in solid flake form is easy to incorporate. It gets quickly dispersed in water at room temperature and hence easily amenable to personal care formulations that are manufactured by cold processing.

(69) 5) The solid easy-to-use preservative composition of the present patent application is compatible with all cosmetic ingredients, stable towards any oxidizing or reducing agents and within the normal range of pH (4.0 to 7.0) of personal care formulations.

(70) 6) The preservative composition of the present invention is suitable for dry forms of home and personal care products like powder face wash or compacts with negligible amount of water.

(71) Anyone with the reasonable level of knowledge of in the art would understand that the solid, easy-to-use, broad spectrum preservative composition of the present invention can be used with additional anti-microbial compounds or adjuvants that can enhance or boost antimicrobial activity synergistically. The examples of such adjuvants are ethylhexyl glyceryl ether, caprylyl glycol, 1,3-Propane diol or EDTA etc.