Patent Description:
The present disclosure relates to preservative compositions for and methods of preserving household formulations, such as detergents, or preserving topical cosmetic or toiletry formulations against microbiological contamination or growth. Specifically, the disclosure relates to preservative compositions comprising an effective amount of a quaternary amine compound, an effective amount of an antifungal, and a solvent. Further, the disclosure relates to cosmetic or toiletry formulations comprising such preservative compositions. The disclosure further relates to method of making and using such preservative compositions and such cosmetic or toiletry formulations comprising the same.

Topical cosmetic and toiletry products such as creams, lotions, pastes, shampoos, gels, wipes and liquid soaps, are known in the art to be susceptible to microbial contaminants. The raw materials, packaging, and manufacturing environment for these products are often not sufficiently sterile, such that microbiological contaminants can enter into final products. Shipment and storage of packaged cosmetic or toiletry products in some cases are performed under uncontrolled conditions. In some cases, a cosmetic or toiletry product may be exposed to higher temperatures than recommended which can also accelerate the growth rate of microbes unless a suitably effective antimicrobial component and/or components are incorporated into the formulation. Once product packages are opened, they are subject to further contamination from repeated consumer use. A consumer may notice microbial infestation by the discoloration and/or unpleasant odor of a product, or they might see macroscopic quantities of microorganisms such as mold on the product. Microbial growth can also cause the degradation of chemical and/or active compounds in the cosmetic or toiletry formulation, which can lead to instability of the product and/or emulsion. A product that has been contaminated by microbiological organisms can also lead to user infections once it is applied to the skin, scalp and/or mucous membranes of a human. It is therefore important for manufacturers and marketers of such products to be able to offer products that resist microbial growth and provide a stable and safe product with a long shelf life.

Typically, topical cosmetic or toiletry manufacturers add small amounts of one or more preservative compounds to their formulations to prevent microbial growth. The preferred preservatives may be water-soluble, since typically it is the water phase of a product that is most susceptible to microbial growth. Preferred preservatives have been those that are effective at use levels and provide cost-effectiveness, and that do not cause excessive irritation, a disadvantage that is associated with some preservative compounds. Preferred preservatives have been those that do not adversely affect the aesthetic properties of the formulation such as the odor and the color. Furthermore, it is also desirable that the preservative does not affect the performance attributes and/or activity of the product.

Preservatives must follow the guidelines established by individual national laws and regulations. In most countries, these regulations limit the type of and use-level of preservatives that may be included in a product. In some countries, certain preservatives are permitted only for rinse-off products (such as shower gels) but not for leave-on products (such as skin creams. ) Therefore, preferred preservatives would be those that are not wholly prohibited in any country, and which are not restricted to only certain product types.

In recent years, cosmetic or toiletry manufacturers have been severely limited in their choice of preservative agents. One class of biocides that has been highly effective in cosmetic or toiletry products includes formaldehyde donors, such as imidazolidinyl urea, diazolidinyl urea, and DMDM hydantoin. However, many such compounds are considered to be skin irritants and the use of formaldehyde donors is severely restricted by regulations in the EU and Japan. Another class of preservatives includes the isothiazolinones, such as methylisothiazolinone (MIT) which is a preservative used in water-based formulations, such as shampoos, liquid soaps, hand lotions and wet wipes. MIT was recently banned by the European Commission in leave-on cosmetic products, and is expected to be further restricted in rinse-off products. Yet another class of preservatives is para-hydroxybenzoic acids, known as parabens. Preservative blends containing parabens are widely used preservative systems. However, research reports such as <NPL>] have suggested that parabens are possible human carcinogens.

Likewise, certain household products, such as fabric softeners, dishwashing liquids having a pH below about <NUM>, all-purpose cleaners having a pH below about <NUM>, and the like, are known in the art to be susceptible to microbial contaminants.

<CIT> describes a preservative composition comprising propylene glycol, benzoic acid, cetylpyridinium chloride and climbazole. The preservative composition is <NUM> to <NUM>% by weight of propylene glycol, <NUM> to <NUM>% by weight benzoic acid %, cetylpyridinium chloride <NUM>-<NUM>% by weight and climbazole <NUM>-<NUM>% by weight.

Because of the recent challenges to traditional preservatives in topical cosmetic and toiletry products, there exists a need to develop novel, economically-viable preservative products that avoid the use of certain components. Likewise, there is a need to develop novel, economically-viable preservative products to preserve household formulations.

In one aspect the present disclosure relates to a preservative composition comprising.

wherein the antifungal agent and the quaternary amine compound are in a ratio of about <NUM>:<NUM> to about <NUM>:<NUM>.

In another aspect the present disclosure relates to a topical cosmetic or toiletry composition comprising.

In a further aspect, the present disclosure relates to a method of preserving a cosmetic or toiletry composition comprising.

In some embodiments, the solvent is selected from the group consisting of propylene glycol, <NUM>,<NUM>-propandiol, glycerin, hexanediol, pentylene glycol, phenoxyethanol, ethylene glycol and benzyl alcohol.

In some embodiments, the cosmetic or toiletry composition is selected from the group consisting of a cream, a lotion, a paste, a shampoo, a gel, a wipe and a liquid soap.

In some embodiments, the surfactant comprises one or more of an anionic surfactant, an amphoteric surfactant, a non-ionic surfactant, or a cationic surfactant.

In some embodiments, the surfactant comprises an anionic surfactant selected from the group consisting of sodium lauryl ether sulfate, sodium lauryl sulfate, ammonium lauryl sulfate, sodium pareth sulfate, sodium lauroyl lactylate, sodium lauryl sulfoacetate, sodium alkyl (C<NUM>-C<NUM>) sulfate and sodium laureth sulfosuccinate.

In some embodiments, the amphoteric surfactant is selected from a group consisting of cocamidopropyl betaine, sodium cocoampoacetate, capryl/capramidopropyl betaine, cocamidopropyl hydroxysultaine, and sodium cocoamphoproprionate.

In some embodiments, the surfactant comprises a non-ionic surfactant selected from the group consisting of PEG-<NUM> cocamide, lauramide DEA/MEA, Cocamide DEA/MEA, decyl glucoside and alkyl polyglucoside.

In some embodiments, the surfactant comprises a cationic surfactant selected from the group consisting of stearalkonium chloride, olealkonium chloride, dipalmitoylethyl hydroxyethylmonium methosulfate, quaternium-<NUM>, a polyquaternium, cetrimonium chloride and PCA ethyl cocoyl arginate.

In some embodiments, the topical cosmetic or toiletry composition further comprises EDTA.

In some embodiments, the preservative composition or the topical cosmetic or toiletry composition is substantially free of methylisothiazolinone.

In some embodiments, the preservative composition or the topical cosmetic or toiletry composition is free of methylisothiazolinone.

As described herein, one aspect of the present disclosure relates to a preservative composition comprising a. an amount of a quaternary amine compound, wherein the quaternary amine compound is about <NUM> wt% to about <NUM> wt% of the preservative composition and wherein the quaternary amine compound is cetyl pyridinium chloride; b. an effective amount of an antifungal agent, wherein the antifungal agent is about <NUM> wt% to about <NUM> wt% of the preservative composition and wherein the antifungal agent is benzoic acid; and c. a solvent; and wherein the antifungal agent and the quaternary amine compound are in a ratio of about <NUM>:<NUM> to about <NUM>:<NUM>.

It will be appreciated that as used herein, "quaternary amine compound" refers to such quaternary ammonium compound (a. quats) as are conventionally known in the art and applicable to the personal care product industry. Such quaternary amine compound can be generally described by the formula NR<NUM>+X-, wherein each R can be independently substituted or unsubstituted alkyl or substituted or unsubstituted aryl, wherein aryl include both all-carbon aromatic groups (such as phenyl or benzyl) and heteroaromatic groups (such as pyridyl), and X-is a suitable counter-ion (or anion).

It will be appreciated that as used herein, "antifungal agent" refers to such agents as are conventionally known in the art and applicable to the personal care product industry. Numerous classes of compounds known in the art have been shown to exhibit antifungal properties, such as imidazole antifungals, triazole antifungals, thiazole antifungals, polyene antifungals, allylamine antifungals, echinocandin antifungals, thiocarbamate antifungals, hydroxypyridone antifungals and antifungal acids.

The preservative compositions and formulations described herein can include one or more booster agents, such as pentylene glycol, caprylyl glycol, and the like. One of skill in the art will readily appreciate that the identity of the booster agent can be one of many known in the art. Furthermore, the identity of a booster can be specific to a given formulation.

A solvent useful in connection with the preservative compositions of the present disclosure can be any solvent known to one of skill in the art that is considered safe and applicable in the personal care product industry. Such solvents include, but are not limited to, propylene glycol, <NUM>,<NUM>-propandiol, glycerin, hexanediol, pentylene glycol, phenoxyethanol, ethylene glycol and benzyl alcohol. In some preferred embodiments, the solvent can be propylene glycol.

It has been surprisingly discovered that the relative proportions of a quaternary amine compound to an antifungal agent in a solvent, all as described above can impact the balance between antimicrobial activity of the resulting preservative composition and the formulation capability of the resulting preservative composition.

In some embodiments, the preservative compositions described herein can be prepared as a concentrate for use in cosmetic or toiletry formulation production. In some embodiments, concentrates of the preservative compositions described herein can be prepared by first dissolving a quaternary amine compound in a solvent as described herein to provide a base concentrate, and then dissolving an antifungal agent as described herein into the base concentrate to provide a preservative composition. In some embodiments, it can be advantageous to warm the solvent to between about <NUM> to about <NUM> prior to dissolving a quaternary amine compound, while stirring the solvent. In some embodiments, it can be advantageous to warm the base concentrate to between about <NUM> to about <NUM> prior to dissolving an antifungal agent, while stirring the base concentrate. In some embodiments, the order of addition of a quaternary amine compound and an antifungal agent can be the reverse of the above description, such that the antifungal agent can be added to a solvent to provide a base concentrate, followed by adding a quaternary amine compound to the base concentrate to provide a preservative composition. In some embodiments, concentrates of the preservative compositions described herein can be prepared by dissolving a quaternary amine compound and an antifungal agent in a solvent as described herein to provide a preservative composition. In some embodiments, it can be advantageous to warm the solvent to between about <NUM> to about <NUM> prior to dissolving a quaternary amine compound and an antifungal agent, while stirring the solvent.

The quaternary amine compound is about <NUM> wt% to about <NUM> wt% of the preservative composition. In some embodiments, the quaternary amine compound can be about <NUM> wt% to about <NUM> wt% of the preservative composition. It will be further appreciated that the present disclosure includes all possible range values of weight% values of the quaternary amine compound within the limits described, such as <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt% and <NUM> wt%. It will be appreciated that as used herein, "wt%" or "weight%" means the mass fraction of a composition as is commonly known in the art. The wt%, mass fraction (wi), is the ratio of one substance with mass (mi) to the mass of the total mixture (mtot), defined as wt% = mi/mtot. One of skill in the art will appreciate that the sum of all mass fractions is equal to <NUM> as <MAT>.

The antifungal agent is about <NUM> wt% to about <NUM> wt% of the preservative composition. In some embodiments, the antifungal agent is about <NUM> wt% to about <NUM> wt% of the preservative composition. It will be further appreciated that the present disclosure includes all possible range values of weight% values of antifungal agent within the limits described, such as <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt% and <NUM> wt%.

In some embodiments, the solvent is about <NUM> wt% to about <NUM> wt% of the preservative composition. In some embodiments, the solvent is about <NUM> wt% to about <NUM> wt% of the preservative composition. It will be further appreciated that the present disclosure includes all possible range values of weight% values of solvent within the limits described, such as <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt% and <NUM> wt%.

In some embodiments, the preservative compositions described herein can be substantially free of methylisothiazolinone. It will be appreciated by one of skill in the art that "substantially free" as used herein means that the amount of methylisothiazolinone is below the minimum amount by weight percent or gross weight allowed by any regulatory agency. By way of non-limiting example, if a regulatory agency allows up to <NUM> wt% of methylisothiazolinone in a personal care product or composition, then "substantially free" for purposes of the present disclosure is less than <NUM> wt%. It will be appreciated that one of skill in the art will understand the limits allowed by regulatory authorities for the use of methylisothiazolinone, and will understand the meets and bounds of "substantially free" based on regulatory requirements commonly known in the art.

In some embodiments, the preservative compositions described herein can be free of methylisothiazolinone. It will be appreciated by one of skill in the art that "free of methylisothiazolinone" as used herein means that the preservative composition does not contain any measurable amount of methylisothiazolinone.

As described herein, one aspect of the present disclosure relates to a topical cosmetic or toiletry composition comprising a. a preservative composition as described herein; and b. at least one surfactant. It will be appreciated that the teachings of present disclosure can be applied to many cosmetic or toiletry compositions known in the art. By way of non-limiting examples, preservative composition as described herein can be used in connection with topical cosmetic or toiletry composition such as creams, lotions, pastes, shampoos, gels, wipes, liquid soaps, and the like. In some embodiments, the preservative composition is in an amount of about <NUM> wt% to about <NUM> wt% of the cosmetic or toiletry composition. It will be further appreciated that the present disclosure includes all possible range values of weight% values of solvent within the limits described, such as <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt% and <NUM> wt%.

It will be appreciated that as used herein, "surfactant" refers to such agents as are conventionally known in the art and applicable to the personal care product industry known to lower the surface tension between two liquids or between a liquid and a solid, and that may act as detergents, emulsifiers, foaming agents or dispersants. It will be appreciated by one of skill in the art that numerous surfactants can be used in connection with the present disclosure. For example, in some embodiments, the surfactant comprises one or more anionic surfactant, non-ionic surfactant, or cationic surfactant. Suitable anionic surfactants include but are not limited to sodium lauryl ether sulfate, sodium lauryl sulfate, ammonium lauryl sulfate, sodium pareth sulfate, sodium lauroyl lactylate, sodium lauryl sulfoacetate, sodium alkyl (C<NUM>-C<NUM>) sulfate and sodium laureth sulfosuccinate. Suitable non-ionic surfactants include but are not limited to PEG-<NUM> cocamide, lauramide DEA/MEA, Cocamide DEA/MEA, decyl glucoside and alkyl polyglucoside. Suitable cationic surfactants include but are not limited to stearalkonium chloride, olealkonium chloride, dipalmitoylethyl hydroxyethylmonium methosulfate, quaternium-<NUM>, a polyquaternium, cetrimonium chloride, lauramidopropyl betaine, cocamidopropyl betaine and PCA ethyl cocoyl arginate.

It will be appreciated that surfactants are typically used in a wide range of concentrations in cosmetic or toiletry compositions and formulations. In some embodiments, the surfactant can be in an amount of about <NUM> to about <NUM> wt% of the cosmetic or toiletry composition. In some embodiments, the surfactant can be in an amount of about <NUM> to about <NUM> wt% of the cosmetic or toiletry composition.

In some embodiments, the cosmetic or toiletry compositions described herein can be substantially free of methylisothiazolinone. It will be appreciated by one of skill in the art that "substantially free" as used herein means that the amount of methylisothiazolinone is below the minimum amount by weight percent or gross weight allowed by any regulatory agency. By way of non-limiting example, if a regulatory agency allows up to <NUM> wt% of methylisothiazolinone in a personal care product or composition, then "substantially free" for purposes of the present disclosure is less than <NUM> wt%. It will be appreciated that one of skill in the art will understand the limits allowed by regulatory authorities for the use of methylisothiazolinone, and will understand the meets and bounds of "substantially free" based on regulatory requirements commonly known in the art.

In some embodiments, the cosmetic or toiletry compositions described herein can be free of methylisothiazolinone. It will be appreciated by one of skill in the art that "free of methylisothiazolinone" as used herein means that the cosmetic or toiletry composition does not contain any measurable amount of methylisothiazolinone.

It will be appreciated that the cosmetic or toiletry compositions described herein can contain other ingredients known in the art as useful in connection with the production such compositions. Suitable examples of other ingredients include, but are not limited to, moisturizer/conditioner, pearlescent pigments, colorants, fragrance, viscosity adjusters and the like. In some embodiments, it can be advantageous to provide cosmetic or toiletry compositions further comprising ethylenediaminetetraacetic acid (EDTA). In some embodiments, the EDTA can be in an amount of <NUM> wt% to about <NUM>. 3wt% of the cosmetic or toiletry composition. It will be appreciated that the EDTA can be added in any wt% described within the stated range including any subrange therein such as, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, <NUM> wt%, and <NUM> wt%.

The pH of a cosmetic or toiletry composition can be a factor in formulation development. It is known in the art that the pH of skin is from about <NUM> to about <NUM>, with typical values in the range of just below <NUM> to just above <NUM>, which provides what is known as the "acid mantle. " (See, for example, <NPL>). The acid mantle is a thin oily film, made up of sweat and sebum, which sits on top of the outmost layer of skin and protects skin from bacteria entering. When bacteria are killed by acid they can't damage the skin but if you strip skin of its acidic mantle by using it becomes much easier for bacteria to find its way in. Our skin's natural acidity neutralizes chemicals and bacteria, which is a necessary part of the body's defense system. The acid mantle can become unbalanced with the use of strong alkaline soaps, cleansers and detergents. As a result, the pH of cosmetic or toiletry compositions is an important design factor in the industry, and this design factor poses challenges to the industry.

For example, typical shampoos have a pH of between <NUM> and <NUM>. Acidic shampoos are the most common type of shampoos. These products typically do not contain soap and their pH is closer to the natural pH of hair. Due to their pH, acidic shampoos do not swell the hair shaft or strip the natural oils. The scales on a hair follicle lay flat at a slightly acidic pH, making the hair feel smooth and look shiny. Gentle shampoo for color-treated hair, for example, aides in bringing hair to its optimal pH level of about <NUM> to help freeze color pigments. This process assists in maintaining color for a longer period of time.

Also by way of example, body wash is typically an emulsion/gel of water and detergent base with added functional ingredients such as moisturizer/conditioner, pearlescent pigments, colorants, fragrance, and the like. Body wash often contains milder surfactant bases than shampoos. In addition to being pH-friendly to the skin (<NUM>-<NUM>), most also contain gentle conditioning agents in the formulation. Body wash typically balances proper detergency against a need to avoid degreasing the skin.

As noted above, the pH requirements of cosmetic or toiletry compositions can create challenges to the industry. Specifically, it is known in the art that the optimum pH for growth of Aspergillus is in the range of about <NUM> to about <NUM> (See, for example, <NPL>). It is also known in the art that numerous most bacterial growth occurs in an environment having a pH range between about pH <NUM> and about <NUM>. It is also known in the art that most fungi, such as yeast and mold, grow best in an environment having a pH range between about pH <NUM> and about <NUM>.

As a result, contamination of cosmetic or toiletry compositions can become a problem over time. Thus the preservation of such cosmetic or toiletry compositions can be an important aspect of product design.

In some embodiments, the cosmetic or toiletry composition has a pH in the range of about <NUM> to about <NUM>. It will be appreciated that the present disclosure includes all possible range values of pH values of the cosmetic or toiletry compositions described herein within the limits described above, such as about <NUM> to about <NUM>, about <NUM> to about <NUM>, about <NUM> to about <NUM>, about <NUM> to about <NUM>, about <NUM> to about <NUM>, about <NUM> to about <NUM>, and the like. It will be appreciated that the pH of any of the preservative compositions as described herein or any of the cosmetic or toiletry compositions described herein can be optionally adjusted by the addition of either a base, such as a solution of NaOH or and acid, such as citric acid, that is compatible with the composition.

An exemplary anionic soap composition as described herein is shown in Table <NUM>.

An exemplary process for the manufacture of the anionic soap composition of Table <NUM> can be provided as follows: <NUM>. Combine Phase A ingredients, with continual mixing, start to heat to <NUM>-<NUM>; <NUM>. Add Phase B ingredients, contiune mixing and heating to between about <NUM> and about <NUM>. Cool composition to between about <NUM> and about <NUM>, and combine the preservative composition of the disclosure, Phase C. Add Phase C to Phase A/B between <NUM>-<NUM> with continued mixing. Adjust the final formulation pH to <NUM>-<NUM> with Phase D ingredients; and <NUM>. Adjust viscosity with Phase E ingredient. It can be advantageous to cool the pH adjusted Phase A/B composition of step <NUM> to about <NUM> to about <NUM> prior to the addition of a preservative composition of the disclosure. It can be advantageous to combine a preservative composition of the disclosure with a portion of the cocamidopropyl betaine for compatibility prior to combining with the pH adjusted Phase A/B composition of step <NUM>.

One of skill in the art will appreciate that the preservative compositions described herein can also be applied to household products. It will be appreciated that the identity of household products known in the art for use in connection with the preservative compositions described herein are not particularly limited, except that the household product should have a pH of below about <NUM>. Examples of household products for use in connection with the preservative compositions described herein include, but are not limited to, fabric softeners, dishwashing liquids having a pH below about <NUM>, all-purpose cleaners having a pH below about <NUM>, and the like.

The formulation of household products useful in connection with the present preservative compositions are not particularly limited. The various components described herein in connection with the preservative compositions can also be used in connection with household products as appropriate. It will be appreciated that certain components specific to household products may also be used. For example, household products can include surfactants, such as, sodium dodecylbenzene sulfonate, sodium toluene sulfonate, TEA lauryl sulfate, and the like.

Any of the preservative compositions described herein can be used in connection with a household product. In some embodiments, the disclosure provides for a household products, such as a fabric softener, a dishwashing liquid having a pH below about <NUM>, and an all-purpose cleaner having a pH below about <NUM> comprising a preservative composition as described herein.

It will be appreciated that as used herein, "a" or "an" carries the meaning of "one or more" in open-ended claims containing the transitional phrase "comprising.

Having described preservative compositions and their use in detail as above, the disclosure will now provide the following examples are for illustrative purposes only. The examples are non-limiting, and are not intended to limit the invention in any way. It will be appreciated by one of skill in the art that modification to the examples provided below are contemplated based on the description and embodiments provided herein.

Samples were prepared according to Table <NUM> for later use in freeze/thaw testing. To prepare samples <NUM> and <NUM>, the stated wt% of cetylpyridinium chloride (CPC) was added to the stated wt% of water and optionally the stated wt% of <NUM>% aqueous SLES solution, optionally followed by the stated wt% of pH adjuster. To prepare samples <NUM>, <NUM>, <NUM> and <NUM>, the preservative composition contained in the test compositions were made by mixing the stated wt% of propylene glycol (PG) with the stated wt% of benzoic acid (BA), followed by warming the base concentrate mixture of propylene glycol and benzoic acid to about <NUM>, then adding the stated wt% of cetylpyridinium chloride (CPC). The preservative composition was then added to a vial containing the stated wt% of water, optionally the stated wt% of a <NUM>% aqueous SLES solution, and optionally the stated wt% of a <NUM>% NaOH or <NUM>% citric acid solution (pH Adj). In Table <NUM>, all amounts shown as wt% are in grams. Table <NUM> shows the initial pH and the final pH of each test sample after addition of the pH adjuster.

Samples were prepared according to Table <NUM> for later use in freeze/thaw testing and/or in biological testing. To prepare samples <NUM>, <NUM>, <NUM> and <NUM>, the stated wt% of cetylpyridinium chloride (CPC) was added to the stated wt% of water and optionally the stated wt% of <NUM>% aqueous SLES solution, optionally followed by the stated wt% of pH adjuster. To prepare samples <NUM>, <NUM>, <NUM> and <NUM>, the stated wt% of propylene glycol (PG) with the stated wt% of cetylpyridinium chloride (CPC), followed by warming the base concentrate mixture of propylene glycol and benzoic acid to about <NUM>, then adding the stated wt% of benzoic acid (BA). The preservative composition was then added to a vial containing the stated wt% of water, the stated wt% of additional propylene glycol, optionally the stated wt% of a <NUM>% aqueous SLES solution, and optionally <NUM>% NaOH or <NUM>% citric acid solution (pH Adj), as needed. In Table <NUM>, all amounts shown as wt% are in grams. Table <NUM> shows the initial pH and the final pH of each test sample after addition of the pH adjuster.

Samples were prepared according to Table <NUM> for later use in freeze/thaw testing. To prepare samples <NUM> and <NUM>, the stated wt% of benzyl alkonium chloride (BAK) was added to the stated wt% of water and optionally the stated wt% of <NUM>% aqueous SLES solution, optionally followed by the stated wt% of pH adjuster. To prepare samples <NUM>, <NUM>, <NUM> and <NUM>, the preservative composition contained in the test compositions were made by mixing the stated wt% of propylene glycol (PG) with the stated wt% of benzoic acid (BA), followed by warming the base concentrate mixture of propylene glycol and benzoic acid to about <NUM>, then adding the stated wt% of benzyl alkonium chloride (BAK). The preservative composition was then added to a vial containing the stated wt% of water, optionally the stated wt% of a <NUM>% aqueous SLES solution, and optionally the stated wt% of a <NUM>% NaOH or <NUM>% citric acid solution (pH Adj). In Table <NUM>, all amounts shown as wt% are in grams. Table <NUM> shows the initial pH and the final pH of each test sample after addition of the pH adjuster.

Each sample vial as prepared in Example <NUM> was subjected to a freeze/thaw challenge where the vial was cooled to -<NUM> until the sample froze solid, then was allowed to warm to room temperature. The presence of solid in the vial was identified before and after one cycle of freeze/thaw. Results are shown in Table <NUM>.

The testing procedure as well as the neutralization efficacy procedure is based upon the "<NPL>. The baseline testing procedure is based upon the "<NPL>.

Test Sample A was prepared according to the procedure described in Example <NUM>(a) using <NUM> wt% of <NUM>% aqueous SLES solution, <NUM> wt% CPC, <NUM> wt% propylene glycol, <NUM> wt% benzoic acid, and <NUM> wt% water. The final pH of the sample composition was <NUM>.

Test Sample B was prepared according to the procedure described in Example <NUM>(a) using 35wt% of <NUM>% aqueous Sodium Lauryl sulfate (SLS) solution, <NUM> wt% CPC, <NUM> wt% propylene glycol, <NUM> wt% benzoic acid, and <NUM> wt% water. The final pH of the sample composition was <NUM>.

Test Sample B was prepared according to the procedure described in Example <NUM>(a) using <NUM>. 4wt% of <NUM>% aqueous SodiumCoceth-30Sulfate solution, <NUM>. 2wt% CPC, <NUM>. 2wt% benzoic acid, <NUM>. 3wt% propylene glycol, <NUM>. 9wt% water. The final pH of the sample composition was <NUM>.

A <NUM> gram sample was diluted into <NUM> of Dey-Engley Broth (D/E) to create a <NUM>:<NUM> dilution and to neutralize antimicrobial properties of the test material. One (<NUM>) mL aliquots of the <NUM>:<NUM> dilution were plated in duplicate. One-tenth (<NUM>) mL aliquots of the <NUM>:<NUM> dilution were also plated to serve as the <NUM>-<NUM> dilution. Plates were poured with Tryptic Soy Agar (TSA) and Sabouraud Dextrose Agar (SDA) to serve as the baseline Aerobic Plate Count (APC) and Yeast and Mold (YM) counts for the study as shown in Table <NUM>.

Neutralization effectiveness streaks were conducted for each sample with the challenged organism. From the <NUM>:<NUM> and <NUM>:<NUM> product dilutions created above (Baseline Test), one (<NUM>) mL aliquots of the <NUM>:<NUM> and <NUM>:<NUM> dilutions were plated for the organism to be challenged. Bacterial plates were poured with TSA and allowed to solidify. Yeast and mold plates were poured with SDA and allowed to solidify. Bacterial, yeast, and mold cultures were prepared and adjusted to yield a suspension at approximately <NUM> x <NUM><NUM> to <NUM> x <NUM><NUM> CFU/mL and diluted to <NUM> x <NUM><NUM> CFU/mL and streaked onto the mold plates. Agar control plates of TSA and SDA were poured and streaked in the same manner. Neutralizer Effectiveness was determined by comparing the growth on the sample to the growth on the agar controls for each test organism/pool of organisms. The neutralizer effectiveness test demonstrated that the media used to conduct the study was suitable for neutralizing the preservative system in the sample at the <NUM>:<NUM> dilution for yeast and mold, and <NUM>:<NUM> for bacteria thereby enabling recovery of viable organisms. In Table <NUM>, "Growth*" means growth of the test organism equivalent in both size and number to that of the control, and "Growth**" means growth of the test organism is not equivalent in size and/or number to that of the control.

An inoculum for each test organism was prepared in <NUM>% Saline to approximately <NUM> x <NUM><NUM> to <NUM> x <NUM><NUM> CFU/mL for bacteria and <NUM> x <NUM><NUM> to <NUM> x <NUM><NUM> CFU/mL for yeasts and mold. Twenty-five (<NUM>) gram aliquots of sample were created for each of the challenge organisms and inoculated individually at a level of <NUM> per <NUM> gram aliquot of product. One (<NUM>) gram samples were removed from each aliquot for enumeration at days <NUM>, <NUM>, <NUM>, <NUM> and <NUM>. Bacterial plates were poured with TSA and incubated at <NUM>-<NUM> for <NUM> days. Yeast and Mold plates were poured with SDA and incubated at <NUM>-<NUM> for <NUM> days. Following incubation, plates were enumerated.

Test Sample D was prepared according to the procedure described in Example <NUM>(a) using <NUM> wt% of <NUM>% aqueous SLES solution, <NUM> wt% CPC, <NUM> wt% propylene glycol, <NUM> wt% benzoic acid, and <NUM> wt% water. The final pH of the soap composition was <NUM>.

Aspergillus brasiliensis (formerly A. niger) - ATCC <NUM>.

A <NUM> gram sample was diluted into <NUM> of Dey-Engley Broth (D/E) to create a <NUM>:<NUM> dilution and to neutralize antimicrobial properties of the test material. One (<NUM>) mL aliquots of the <NUM>:<NUM> dilution were plated in duplicate. One-tenth (<NUM>) mL aliquots of the <NUM>:<NUM> dilution were also plated to serve as the <NUM>-<NUM> dilution. Plates were poured with Sabouraud Dextrose Agar (SDA) to serve as the baseline Mold (YM) counts for the study. (<<NUM> X <NUM><NUM>).

Neutralization effectiveness streaks were conducted for each sample with the challenged organism. From the <NUM>:<NUM> and <NUM>:<NUM> product dilutions created above (Baseline Test), one (<NUM>) mL aliquots of the <NUM>:<NUM> and <NUM>:<NUM> dilutions were plated for the organism to be challenged. Mold plates were poured with SDA and allowed to solidify. Mold cultures were prepared and adjusted to yield a suspension at approximately <NUM> x <NUM><NUM> to <NUM> x <NUM><NUM> CFU/mL and diluted to <NUM> x <NUM><NUM> CFU/mL and streaked onto the mold plates. Agar control plates SDA were poured and streaked in the same manner. Neutralizer Effectiveness was determined by comparing the growth on the sample to the growth on the agar controls for the test organism. The neutralizer effectiveness test demonstrated that the media used to conduct the study was suitable for neutralizing the preservative system in the sample at the <NUM>:<NUM> dilution for mold thereby enabling recovery of viable mold organisms. In Table <NUM>, "Growth*" means growth of the test organism equivalent in both size and number to that of the control.

An inoculum for the test organism was prepared in <NUM>% Saline to approximately <NUM> x <NUM><NUM> to <NUM> x <NUM><NUM> CFU/mL for mold. A twenty-five (<NUM>) gram aliquot of sample was created for the challenge organism and was inoculated at a level of <NUM> per <NUM> gram aliquot of product. One (<NUM>) gram samples were removed from the aliquot for enumeration at days <NUM>, <NUM>, <NUM>, and <NUM>. Mold plates were poured with SDA and incubated at <NUM>-<NUM> for <NUM> days. Following incubation, plates were enumerated.

Claim 1:
A preservative composition comprising
a. an amount of a quaternary amine compound, wherein the quaternary amine compound is about <NUM> wt% to about <NUM> wt% of the preservative composition and wherein the quaternary amine compound is cetyl pyridinium chloride;
b. an effective amount of an antifungal agent, wherein the antifungal agent is about <NUM> wt% to about <NUM> wt% of the preservative composition and wherein the antifungal agent is benzoic acid; and
c. a solvent; and
wherein the antifungal agent and the quaternary amine compound are in a ratio of about <NUM>:<NUM> to about <NUM>:<NUM>.