Patent Description:
Many antiperspirant and deodorants use actives that are astringent metallic salts, or in particular, aluminum salts. While aluminum is highly effective as an active, there is consumer interest in antiperspirants and deodorants that do not contain aluminum.

Consumers are also seeking more natural products complete with fragrances that are mostly natural or essential oil based. They are further seeking products with lower irritation than they have experienced with baking soda based products. The challenge with formulating with the natural and essential oil fragrances is that they can be less stable in the presence of heat and extreme pH (either high or low). And products formulated with baking soda, which has a relatively high pH and high water solubility, can increase irritation, even for consumers with moderate sweat rates. Highly water soluble alkaline powders contribute negatively towards natural or essential oil stability as well, especially in a hot process needed to melt waxes. And high water solubility powders can also lead to gritty products, as the water soluble powders can agglomerate when exposed to moisture released from powders during the hot batch process.

<CIT> refers to a composition in which the volatile silicone is partially or fully replaced by a plant oil.

<CIT> is about formulations all commonly including magnesium oxide, zinc oxide and as a disinfecting agent, potassium chloride and/or potassium sulphate.

<CIT> sets out a composition that is gelled with a high level of fatty acid.

<CIT> is related to anhydrous antiperspirant and deodorant compositions comprising from <NUM> % to <NUM>% by weight of an underarm active (antiperspirant and/or deodorant active); from <NUM> % to <NUM>% by weight of a solid, encapsulated, water-soluble, d-pantothenate salt such as calcium pantothenate; from <NUM> % to <NUM>% by weight of a suspending agent; and from <NUM>% to <NUM>% by weight of an anhydrous carrier liquid.

"<NPL>) has an all-natural formula that is claimed to effectively neutralize underarm odor and absorb wetness.

Thus, here is a continuing challenge to formulate a non-aluminum, natural fragrance deodorant that provides low irritation while maintaining sufficient odor protection.

Piroctone olamine is an anti-dandruff active used in shampoos, conditioners, and other treatments. Piroctone olamine can be an effective antimicrobial, but used alone as an active, it may not deliver the hoped for consumer performance. The inventors of the present invention have found, surprisingly, that the combination of piroctone olamine and other antimicrobials can provide significant antimicrobial activity against two of the most common underarm odor bacteria C. mucofaciens and S. epidermidis, which results in consumer odor protection on par or greater than some of the commonly used commercial deodorants available today.

Also to consider is that impurities can reduce the efficacy of piroctone olamine. Therefore, there is a need to develop products that mitigate this phenomenon and provide higher efficacy. The inventors of the present invention have found that select combinations of chelators and piroctone olamine, such as in an anhydrous formulation or in particular ratios, can provide significantly higher levels of anti-fungal activity than either material alone.

Furthermore, while antimicrobials in antiperspirants and deodorants are known to be able to reduce the microbes on the skin, microbes within hair follicles may still remain and contribute to malodor. The inventors of the present invention have found that piroctone olamine and other antimicrobial powders, if used at a size that can fit into a hair follicle, can deliver surprisingly superior antimicrobial activity.

By utilizing piroctone olamine in combination with appropriate antimicrobials, chelators, and/or at particular particle sizes, the present invention delivers compositions and products with superior antimicrobial performance.

A deodorant stick comprising at least <NUM>% of a liquid triglyceride, wherein the triglyceride is liquid at <NUM>, wherein the liquid triglyceride is caprylic/capric triglyceride, wherein the total amount of liquid triglyceride is at least <NUM>% by weight; a primary antimicrobial having a water solubility of at most <NUM>/L at <NUM>; a fragrance composition comprising at least <NUM>% natural oils, essential oils, or a combination thereof; and a primary structurant with a melting point of at least <NUM>, wherein the primary structurant is ozokerite; said deodorant stick being free of an aluminum salt; and said deodorant stick having a hardness from <NUM> (<NUM>*<NUM>) to <NUM> (<NUM>*<NUM>), as measured by penetration with ASTM D-<NUM> needle.

While the specification concludes with claims that particularly point out and distinctly claim the invention, it is believed the present invention will be better understood from the following description.

The present invention can comprise, consist of, or consist essentially of the essential elements and limitations of the invention described herein, as well any of the additional or optional ingredients, components, or limitations described herein.

All percentages, parts and ratios are based upon the total weight of the compositions of the present invention, unless otherwise specified. All such weights as they pertain to listed ingredients are based on the active level and, therefore do not include carriers or by-products that may be included in commercially available materials.

The components and/or steps, including those which may optionally be added, of the various embodiments of the present invention, are described in detail below.

All ratios are weight ratios unless specifically stated otherwise.

All temperatures are in degrees Celsius, unless specifically stated otherwise.

Except as otherwise noted, the articles "a", "an", and "the" mean "one or more".

Herein, "comprising" means that other steps and other ingredients which do not affect the end result can be added. The compositions and methods/processes of the present invention can comprise, consist of, and consist essentially of the essential elements and limitations of the invention described herein, as well as any of the additional or optional ingredients, components, steps, or limitations described herein.

Herein, "effective" means an amount of a subject active high enough to provide a significant positive modification of the condition to be treated. An effective amount of the subject active will vary with the particular condition being treated, the severity of the condition, the duration of the treatment, the nature of concurrent treatment, and like factors.

The term "anhydrous" as used herein means substantially free of added or free water. From a formulation standpoint, this means that the anhydrous antiperspirant or deodorant stick compositions of the present invention contain less than <NUM>%, and more specifically zero percent, by weight of free or added water, other than the water of hydration typically associated with the particulate antiperspirant or deodorant active prior to formulation.

The term "ambient conditions" as used herein refers to surrounding conditions under one atmosphere of pressure, at <NUM>% relative humidity, and at <NUM>, unless otherwise specified. All values, amounts, and measurements described herein are obtained under ambient conditions unless otherwise specified.

The term "majority" refers to greater than <NUM>% of the stated component or parameter.

The term "polarity" as used herein is defined by the Hansen Solubility Parameter for solubility.

"Substantially free of" refers to <NUM>% or less, <NUM>% or less, or <NUM>% or less of a stated ingredient. "Free of" refers to no detectable amount of the stated ingredient or thing.

The term "volatile" as used herein refers to those materials that have a measurable vapor pressure at <NUM>. Such vapor pressures typically range from <NUM> millimeters of Mercury (mm Hg) to <NUM> mmHg, more typically from <NUM> mmHg to <NUM> mmHg; and have an average boiling point at one (<NUM>) atmosphere of pressure of less than <NUM>, more typically less than <NUM>. Conversely, the term "non-volatile" refers to those materials that are not "volatile" as defined herein.

<NUM>-Pyridinol-N-oxide materials suitable for use in this invention include a substituted or unsubstituted <NUM>-pyridinol-N-oxide material or a salt thereof. Included within the scope of this invention are tautomers of this material, e.g., <NUM>-hydroxy-<NUM>(<NUM>)-pyridinone. The substituted or unsubstituted <NUM>-pyridinol-N-oxide material and its corresponding tautomeric form, <NUM>-hydroxy-<NUM>(<NUM>)-pyridinone, are shown below:
<CHM>
where R<NUM>, R<NUM>, R<NUM>, R<NUM> groups are independently selected from the group consisting of H, Cl, Br, I, F, NO, NO<NUM>, and (CH<NUM>)nG, where each G is independently selected from the group consisting of (O)mSO<NUM>M<NUM>, (O)mCO<NUM>M<NUM>, (O)mC(O)(R<NUM>), (O)mC(O)N(R<NUM>R<NUM>), (O)mCN, (O)m(R<NUM>), and N(R<NUM>R<NUM>), where m is <NUM> or <NUM>, n is an integer from <NUM> to <NUM>, R<NUM> and R<NUM> are independently selected from the group consisting of H and a substituted or unsubstituted C<NUM>-C<NUM> organic group, and M<NUM> is selected from the group consisting of H, a substituted or unsubstituted C<NUM>-C<NUM> organic group, +N(R<NUM>R<NUM>R<NUM>R<NUM>), and <NUM>/q M' q+ where M' is selected from the group consisting of an alkali metal of charge q and an alkaline earth metal of charge q, where R7, R8, R9, and R10 are independently selected from the group consisting of H and a substituted or unsubstituted C<NUM>-C<NUM> organic group, and where any pair of vicinal groups, R<NUM> and R<NUM>, R<NUM> and R<NUM>, R<NUM> and R<NUM> may be taken together to form another five- or six-membered aromatic or aliphatic ring optionally substituted with one or more groups selected from the group consisting of Cl, Br, I, F, NO, NO<NUM>, CN, (CH<NUM>)nG, and mixtures thereof. Suitable organic groups include (C<NUM>-C<NUM>)alkyl, (C<NUM>-C<NUM>)alkenyl, and (C<NUM>-C<NUM>)alkynyl. The organic group may optionally be substituted and suitable substituent groups include a hydroxyl group, a carboxyl group, and an amino group. <NUM>-pyridinol-N-oxide is also known, for example, as <NUM>-hydroxypyridine-N-oxide, <NUM>-pyridinol-<NUM>-oxide, or <NUM>-hydroxypyridine-<NUM>-oxide.

In certain aspects, the <NUM>-pyridinol-N-oxide material is a <NUM>-pyridinol-N-oxide material or tautomer thereof according to the formula(s) above, where R<NUM>, R<NUM>, R<NUM>, R<NUM> are independently selected from the group consisting of H, Cl, and (CH<NUM>)nG, where G is independently selected from the group consisting of (O)mSO<NUM>M<NUM>, (O)mCO<NUM>M<NUM>, (O)mC(O)(R<NUM>), (O)mCN, and (O)m(R<NUM>), where m is <NUM> or <NUM>. In other aspects, the <NUM>-pyridinol-N-oxide material is a <NUM>-pyridinol-N-oxide material according to the formula above, where R<NUM>, R<NUM>, R<NUM>, R<NUM> are independently selected from the group consisting of H, SO<NUM>M<NUM>, and CO<NUM>M<NUM>. In still other aspects, R<NUM>, R<NUM>, R<NUM>, R<NUM> are independently selected from the group consisting of H, SO<NUM>M<NUM>, and CO<NUM>M<NUM>, where no more than one R<NUM>, R<NUM>, R<NUM>, R<NUM>is SO<NUM>M<NUM> or CO<NUM>M<NUM>.

In certain aspects, the <NUM>-pyridinol-N-oxide material is the salt of a substituted or unsubstituted <NUM>-pyridinol-N-oxide material. In these aspects, the hydrogen of the hydroxyl group of the <NUM>-pyridinol-N-oxide material may be substituted with a suitable charge-balancing cation. In these aspects, non-limiting examples of the hydrogen-substituting cation include Na+, Li+, K+, ½ Mg<NUM>+, or ½ Ca<NUM>+, substituted ammonium, such as C<NUM>-C<NUM> alkanolammnonium, mono-ethanolamine (MEA), tri-ethanolamine (TEA), di-ethanolamine (DEA), or any mixture thereof. In some aspects, in solution, the cation may be dissociated from the <NUM>-pyridinol-N-oxide or the <NUM>-hydroxy-<NUM>(<NUM>)-pyridinone anion.

In certain aspects, the <NUM>-pyridinol-N-oxide material is of a substituted or unsubstituted <NUM>-pyridinol-N-oxide material. Salts for use herein include those formed from the polyvalent metals barium, bismuth, strontium, copper, zinc, cadmium, zirconium and mixtures thereof.

In some aspects, the <NUM>-pyridinol-N-oxide material is selected from the group consisting of: <NUM>-hydroxy-<NUM>-pyridinesulfonic acid, <NUM>-oxide <NPL>); <NUM>-hydroxypyridine-<NUM>-oxide (<NPL>); <NUM>-hydroxy-<NUM>-pyridinecarboxylic acid, <NUM>-oxide (<NPL>); <NUM>-ethoxy-<NUM>-pyridinol, <NUM>-acetate, <NUM>-oxide (<NPL>); <NUM>-(<NUM>-hydroxy-<NUM>-oxido-<NUM>-isoquinolinyl)-ethanone (<NPL>); <NUM>-hydroxy-<NUM>-pyridinecarboxylic acid, <NUM>-oxide (<NPL>); <NUM>-methoxy-<NUM>-quinolinecarbonitrile, <NUM>-oxide (<NPL>); <NUM>-pyridinecarboxylic acid, <NUM>-hydroxy-, <NUM>-oxide (<NPL>); <NUM>-pyridinecarboxylic acid, <NUM>-hydroxy-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>-nitro-, <NUM>-oxide (<NPL>); <NUM>-pyridinepropanenitrile, <NUM>-hydroxy-, <NUM>-oxide (<NPL>); <NUM>-pyridineethanol, <NUM>-hydroxy-, <NUM>-acetate, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>-bromo-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>,<NUM>-dibromo-, <NUM>-acetate, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>,<NUM>-dibromo, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>-(<NUM>-aminoethyl)-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>-(<NUM>-aminoethyl)-, <NUM>-oxide (<NPL>); <NUM>-pyridinepropanoic acid, α-amino-<NUM>-hydroxy-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>,<NUM>-dimethyl, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>-methyl-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>,<NUM>-dinitro, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>,<NUM>-dibromo-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>-methyl-<NUM>-(<NUM>-methylpropyl)-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>-bromo-<NUM>,<NUM>-dimethyl-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>,<NUM>,<NUM>-trimethyl-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>-heptyl-<NUM>-methyl-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>-(cyclohexylmethyl)-<NUM>-methyl-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>-bromo-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>-bromo-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>,<NUM>-dichloro-<NUM>,<NUM>-difluoro-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>,<NUM>,<NUM>,<NUM>-tetrachloro-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>-methyl-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>-nitro-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>-methyl-<NUM>-nitro-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>-chloro-<NUM>-nitro-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>-chloro-, <NUM>-oxide (<NPL>); <NUM>-pyridinol, <NUM>-nitro-, <NUM>-oxide (<NPL>); and <NUM>-pyridinol, <NUM>-methyl-, <NUM>-oxide (<NPL>), and mixtures thereof. These materials are commercially available from, for example, Sigma-Aldrich (St. Louis, MO) and/or Aces Pharma (Branford, CT).

In certain aspects, the <NUM>-pyridinol-N-oxide material is a <NUM>-pyridinol-N-oxide material selected from the group consisting of: <NUM>-hydroxypyridine-<NUM>-oxide; <NUM>-pyridinecarboxylic acid, <NUM>-hydroxy-, <NUM>-oxide; <NUM>-hydroxy-<NUM>-pyridinecarboxylic acid, <NUM>-oxide; <NUM>-hydroxy-<NUM>-pyridinecarboxylic acid, <NUM>-oxide; <NUM>-pyridinecarboxylic acid, <NUM>-hydroxy-, <NUM>-oxide; <NUM>-hydroxy-<NUM>-pyridinesulfonic acid, <NUM>-oxide; and mixtures thereof.

In certain aspects, the <NUM>-pyridinol-N-oxide material is a <NUM>-Hydroxy-<NUM>(<NUM>)-pyridinone material selected from the group consisting of: <NUM>-Hydroxy-<NUM>(<NUM>)-pyridinone (<NPL>dihydro-<NUM>-hydroxy-<NUM>-oxo-<NUM>-Pyridinecarboxylic acid (<NPL>); <NUM>,<NUM>-dihydro-<NUM>-hydroxy-<NUM>-oxo-<NUM>-Pyridinecarboxylic acid (<NPL>); <NUM>,<NUM>-dihydro-<NUM>-hydroxy-<NUM>-oxo-<NUM>-Pyridinecarboxylic acid (<NPL>); <NUM>-hydroxy-<NUM>-methyl-<NUM>-(<NUM>,<NUM>,<NUM>-trimethylpentyl)-<NUM>(<NUM>)-Pyridinone (<NPL>); <NUM>-(cyclohexylmethyl)-<NUM>-hydroxy-<NUM>-methyl-<NUM>(<NUM>)-Pyridinone (<NPL>); <NUM>-hydroxy-<NUM>,<NUM>-dimethyl-<NUM>(<NUM>)-Pyridinone (<NPL>); <NUM>-Hydroxy-<NUM>-methyl-<NUM>-(<NUM>,<NUM>,<NUM>-trimethylpentyl)-<NUM>-pyridone monoethanolamine (<NPL>; <NUM>-hydroxy-<NUM>-(octyloxy)-<NUM>(<NUM>)-Pyridinone (<NPL>); <NUM>-Hydroxy-<NUM>-methyl-<NUM>-cyclohexyl-<NUM>-pyridinone ethanolamine salt (<NPL>); <NUM>-Hydroxy-<NUM>-methyl-<NUM>-cyclohexyl-<NUM>-pyridinone (<NPL>); <NUM>-ethoxy-<NUM>,<NUM>-dihydro-<NUM>-hydroxy-<NUM>-oxo-<NUM>-Pyridinecarboxylic acid,methyl ester (<NPL>); <NUM>-hydroxy-<NUM>-nitro -<NUM>(<NUM>)-Pyridinone (<NPL>); and mixtures thereof. These materials are commercially available from, for example, Sigma-Aldrich (St. Louis, MO), Princeton Building Blocks (Monmouth Junction, NJ), 3B Scientific Corporation (Libertyville, IL), SynFine Research (Richmond Hill, ON), Ryan Scientific, Inc. Pleasant, SC), and/or Aces Pharma (Branford, CT).

In certain aspects, the <NUM>-pyridinol-N-oxide material is a <NUM>-pyridinol-N-oxide material or tautomer thereof according to the formula(s) below:
<CHM>
where X is an oxygen or sulfur moiety and R is a substituted or unsubstituted hydrocarbon group having between <NUM> and <NUM> carbon atoms. Materials of this class can be synthesized following the procedure disclosed in <CIT>.

In certain aspects, the <NUM>-pyridinol-N-oxide material is a <NUM>-pyridinol-N-oxide material or tautomer thereof according to the formula(s) below:
<CHM>.

Wherein R' and R" are independently either hydrogen or a substituted or unsubstituted hydrocarbon group having between <NUM> and <NUM> carbon atoms. Materials of this class can be synthesized following the procedure disclosed in <CIT>. In certain aspects, the <NUM>-pyridinol-N-oxide material is <NUM>-Hydroxy-<NUM>-methyl-<NUM>-(<NUM>,<NUM>,<NUM>-trimethylpentyl)-<NUM>-pyridone monoethanolamine salt.

The amount of <NUM>-pyridinol-N-oxide (which may throughout this disclosure sometimes be referred to as piroctone olamine) in antiperspirant or deodorant formulations of the present invention may be from <NUM>% to <NUM>% by weight, in some embodiments from <NUM>% to <NUM>% by weight, and in some embodiments from <NUM>% to <NUM>% by weight.

In the present invention, iron chelators may have, but are not limited to, the following characteristics:.

In an embodiment of the present invention, an iron chelator may be present from the following groups:.

Specific and/or additional chelators in the present invention may include, but are not limited to, diethylenetriaminepentaacetic acid (DTPA), diethylenetriaminepentakis (methylenephosphonic acid) (DTPMP), desferrioxamine, their salts and combinations thereof, EDTA, DPTA, EDDS, enterobactin, desferrioxamine, HBED, and combinations thereof.

While piroctone olamine can be an effective antimicrobial for an antiperspirant or deodorant, the presence of iron and other impurities may reduce piroctone olamine's effectiveness. As such, the inventors of the present invention have found that including a chelant to bond with iron, for example, can reduce the occurrence of piroctone olamine itself bonding with the iron, essentially freeing the piroctone olamine to be effective against bacteria.

This is particularly true in anhydrous formulations. In an aqueous formulation comprising piroctone olamine and a chelant, the chelant can improve piroctone olamine's efficacy because the chelant should have more affinity for the iron than the piroctone olamine has affinity for the iron. In addition, in an anhydrous formulation, with little or no water, the water solubility of the materials comes into play when sweat meets the formulation. Piroctone olamine typically has a lower water solubility than a chelant, meaning that in an anhydrous formulation, the chelant's higher water solubility results in the chelant more quickly getting into solution and bonding with iron, i.e., before the piroctone olamine gets into solution. This further advantage only exists in an anhydrous formulation, as in an aqueous formulation, everything is fully in solution from the beginning.

Table <NUM> below shows the intrinsic water solubility independent of pH (LogWSo) of piroctone olamine and EDTA as an example. The lower LogWSo of piroctone olamine indicates that it will get into solution more slowly than a chelant such as EDTA, and the chelant will have more of an opportunity to bond with iron than the piroctone olamine will.

Furthermore, the inventors of the present invention have found that the ratio of chelant to piroctone olamine may be important. In some embodiments, the improved efficacy of a chelant with piroctone olamine can be seen when the ratio of chelant to piroctone is at least <NUM>:<NUM>, in some embodiments at least <NUM>:<NUM>, and in some embodiments, at least <NUM>:<NUM>. The amount of chelant, by weight of composition, may be from <NUM>% to <NUM>%.

The present inventors have discovered that the water solubilities of certain components in the solid stick antiperspirant or deodorant have great importance. Some deodorant ingredients will bring in moisture to the batch, which can solvate these components to different extents when the water evaporates and subsequently recondenses as free water in the batch. Certain batch processing conditions (such as a closed top on the tank) could more effectively trap this water in the tank, where it is then free to interact with components of the batch. For example, highly water soluble alkaline powders can contribute negatively towards natural and essential oil stability when dissolved. This is because many natural and essential oils contain a broad range of perfume chemicals, many of which can undergo degradation reactions when exposed to extreme pH or heat. This is why many natural and essential oils have shorter shelf lives than many commercial synthetic chemicals or perfumes. And certain antimicrobials may cause irritation due to high water solubility. Further, high water solubility can lead to grittier products as the more water soluble powders can agglomerate when exposed to moisture released from powders during the heat of manufacture.

To demonstrate this concept, the present inventors made two batches of deodorant product following the same formula, where baking soda (high water solubility) was the active ingredient. The fragrance contained <NUM>-<NUM>% natural vanilla. Batch A was made similarly to the inventive formulas herein. Batch B had <NUM>% water added into the batch during cooling to simulate moisture that could evaporate and recondense in a tank under certain process conditions. The differences in Batch B were almost immediately obvious. The color of the batch became a deep brown during a brief hold time of <NUM> minutes.

As previously explained, it is believed that the water solvates the baking soda since it is so highly water soluble, and the resulting high pH solution degrades fragrance (particularly the more susceptible natural vanilla). The resulting byproducts change the color and odor of the batch.

Color and odor were observed to be adversely affected by the excess water. The color difference was very visually obvious. The odor differences were confirmed with an odor panel, in which the comparison of Batch A (control) vs. Batch B failed with a grade of <NUM> (below <NUM> is a failure). Thus, embodiments of the present invention may include an antimicrobial with a low water solubility. An antimicrobial with a low water solubility may be, in some embodiments, an antimicrobial with a water solubility of at most <NUM>/L at <NUM>, in other embodiments at most <NUM>/L at <NUM>, or in still other embodiments at most <NUM>/L at <NUM>.

Materials with a water solubility above <NUM>/L @<NUM> include but are not limited to: potassium carbonate, potassium bicarbonate, sodium carbonate, sodium sesquicarbonate, triethyl citrate, and baking soda. Materials with a water solubility below <NUM>/L @<NUM> include but are not limited to: beryllium carbonate, magnesium carbonate, calcium carbonate, magnesium hydroxide, magnesium hydroxide and magnesium carbonate hydroxide, partially carbonated magnesium hydroxide, piroctone olamine, hexamidine, zinc carbonate, thymol, polyvinyl formate, salicylic acid, phenoxyethanol, eugenol, linolenic acid, dimethyl succinate, citral, and triethyl citrate. Each of beryllium carbonate, magnesium carbonate, calcium carbonate, magnesium hydroxide, magnesium hydroxide and magnesium carbonate hydroxide, partially carbonated magnesium hydroxide, piroctone olamine, hexamidine, zinc carbonate, thymol, polyvinyl formate, salicylic acid, phenoxyethanol, eugenol, linolenic acid, dimethyl succinate, and citral have a water solubility below <NUM>/L @<NUM>, below <NUM>/L @<NUM>, below <NUM>/L @<NUM>, and below <NUM>/L @<NUM>.

As <FIG> shows, when samples of a deodorant product containing partially carbonated magnesium hydroxide (low water solubility) and a deodorant product containing baking soda (high water solubility) were put through a humidity ramp from <NUM>% relative humidity (RH) to <NUM>% RH and back to <NUM>% RH, the baking soda deodorant gained and lost more water weight than the partially carbonated magnesium hydroxide deodorant. Absorbing more water puts the product at risk of grittiness and perfume instability.

For example, the data below shows one product difference when using high vs. low water solubility powders. Product A, with a low water solubility antimicrobial powder, demonstrated better perfume stability than Product B, which had a high water solubility antimicrobial powder:.

Odor grading was completed on a solid stick deodorant containing a low water solubility powder of magnesium hydroxide & magnesium carbonate hydroxide (Product A), as well as a solid stick deodorant containing a high water solubility powder of baking soda (Product B). Both products had the same level of a fragrance, which was composed entirely of natural and essential oils. Jars containing samples of the products were heated at <NUM> for <NUM>, <NUM>, and <NUM> days as part of a rapid stability program. All odor grades were made for the heated jars in comparison to a control, which was an unheated jar of product A. The grades evaluate scent character and intensity changes. If at any time point there is an average odor grade score below a <NUM>, the product is considered an odor grade failure. The product containing the high water solubility powder failed odor grading, while the product with the low water solubility passed odor grading. This serves as an example of how natural and essential oil blends would be more susceptible to degradation and less stability when used with high water solubility powders.

The present invention may include one or more antimicrobial compositions. For example, antimicrobials may include, without being limited to, piroctone olamine, hexamidine, magnesium carbonate, zinc carbonate, thymol, magnesium hydroxide, dead sea salt, magnesium hydroxide and magnesium carbonate hydroxide, partially carbonated magnesium hydroxide, calcium carbonate, polyvinyl formate, salicylic acid, niacinamide, phenoxyethanol, eugenol, linolenic acid, dimethyl succinate, citral, triethyl citrate, sepiwhite, baking soda, partially carbonated magnesium hydroxide, magnesium carbonate hydroxide, cinnamon essential oil, cinnamon bark essential oil, cinnamic aldehyde, and combinations thereof.

In general, the total amount of antimicrobial used in the present invention may be from <NUM>% to <NUM>%, by weight, of the deodorant. Some antimicrobials may be used in amounts as low as <NUM>%, by weight of the deodorant, such as if using piroctone olamine or hexamidine as the primary antimicrobial, while others could be as high as <NUM>%, such as if using magnesium hydroxide or magnesium hydroxide and magnesium carbonate hydroxide as the primary antimicrobial (primary antimicrobial being the antimicrobial present in the composition in the highest amount). In the latter cases, baking soda might still be used at a lower level, such as from <NUM>% to <NUM>%, as a secondary antimicrobial, or not at all.

Any of the antimicrobials of the present invention may be used as powders. It is believed that antimicrobial powders may provide a better deposition and have more longevity on the skin than antimicrobials delivered in a different form. In addition, it is believed that antimicrobial powders of a certain average particle size, typically from <NUM> micron to <NUM> microns, may provide a significant increase in antimicrobial efficacy.

Many antimicrobials can be effective at minimizing the skin surface bacteria. However, as a leave-on product where odor may not occur until later, even hours after application, antiperspirant and deodorant antimicrobials are needed that will be effective for long periods of time. So while antiperspirant and deodorant antimicrobials may be effective immediately upon application on the skin, it is believed that odor comes back quickly because the bacteria living around the hair follicle can quickly repopulate the skin surface bacteria. Historical approaches using high skin penetrating liquid antimicrobials to affect this region (for example, hexanediol) can cause irritation. Therefore, the present invention is able to target methods and mechanisms that can more effectively deliver antimicrobials not only to the skin surface, but to the bacteria in and around the hair follicle. While not wanting to be bound to the theory, the inventors of the present invention believe that powders, specifically powders with an average particle size of less than <NUM> microns, in some cases from <NUM> micron to <NUM> microns, are more efficient at getting into the hair follicle where the bacteria live and repopulate the skin surface.

As shown in <FIG> and <FIG>, a hair <NUM> is partly above the skin surface and partly below the skin surface in the hair follicle <NUM>. The antimicrobial particles, <NUM> and <NUM>, upon application, may be on the surface of the skin at the skin secretion/air/sweat interface <NUM> and where there is bacteria <NUM>. As shown in <FIG> and <FIG>, the sebaceous gland <NUM> and the apocrine gland <NUM> in the skin have secretions that are in the hair follicle <NUM>. Bacteria <NUM> and odor precursors <NUM> are embedded in the secretions. In <FIG>, the larger antimicrobial particles <NUM> are too big to fit into the hair follicle, leaving the secretions inside the hair follicle untouched. The antimicrobial particles <NUM> come in contact with bacteria only on the surface of the skin. In <FIG>, however, the antimicrobial particles <NUM> are sized to fit within the hair follicle and deliver antimicrobial activity not only to the surface of the skin, but also directly and immediately to the hair follicle secretions <NUM> and <NUM>. Having the antimicrobial particles be in the range of <NUM> to <NUM> microns, in some embodiments <NUM> to <NUM> microns, provides better odor protection later in the day hours after application of the antiperspirant or deodorant when other good antimicrobial materials and other sizes of antimicrobial materials are not as effective against this rebound in bacteria population from the follicle.

Table <NUM> below shows the raw material microbial inhibition concentration data tested against two key underarm bacteria strains. As can be seen, the first three listed antimicrobials, lupamin, hexamidine, and piroctone olamine, perform particularly well against the bacteria as raw materials. Also performing well as raw materials are phenoxyethanol, eugenol, linolenic acid, dimethyl succinate, citral, triethyl citrate, and sepiwhite. Also performing moderately well against the bacteria as raw materials were magnesium carbonate and magnesium hydroxide and calcium carbonate.

While numerous antimicrobials exhibit efficacy against two main bacteria strains that antiperspirants and deodorants try to address, due to regulatory and safety reasons, there are sometimes limits as to how much of a particular antimicrobial may be put into an antiperspirant or deodorant formula. Therefore, there is a need for multiple antimicrobials to work together in a formula to deliver enough long-term odor protection. The inventors of the present invention believe that piroctone olamine may be an ideal antimicrobial to combine with other antimicrobials.

Table <NUM> is a summary of in-use consumer data for Inventive Formulas <NUM>-<NUM> shown in Table <NUM> along with a comparative deodorant that is a currently marketed aluminum-free product with a high water solubility active (baking soda). As seen in Table <NUM>, the inventive formulas produce a consumer-accepted deodorant that works on par with the high water solubility deodorant. And as discussed herein, the use of the low water solubility actives can provide additional perfume stability and aesthetic benefits that deodorants with high water solubility actives cannot. Consumer data test method: Phase <NUM> was four days of soap washing only (no underarm product use). Both phase <NUM> and <NUM> included once per day application of test products for eight days. The desired dose was <NUM>. Subjects were asked to complete twice daily self-assessed odor evaluations and once daily discomfort evaluation.

The strength of the association between a ligand and metal, in this case iron, can be termed iron affinity. A high iron binding affinity is required for chelators to effectively compete with iron salt impurities that reduce the efficacy of <NUM>-pyridinol-N-oxide materials.

Affinity between a metal (M) and ligand (L) can be measured by the stepwise association constant, K<NUM> which describes the following equilibrium: <MAT>.

The affinity constant is conveniently expressed as the logarithm (log K<NUM>) and the larger the magnitude of this number, the stronger the association between the metal (iron ions in this case) and ligand.

In an embodiment of the present invention, the antiperspirant or deodorant composition may contain an iron chelator which has a log K<NUM> greater than <NUM>. In a further embodiment, the antiperspirant or deodorant composition may contain an iron chelator which has a log K<NUM> greater than <NUM>.

The antiperspirant and/or deodorant compositions (for simplicity sometimes referred to as either antiperspirant or deodorant compositions) as described herein contain a primary structurant, an antiperspirant active, a perfume, and additional chassis ingredient(s), as claimed in present claim <NUM>. The antiperspirant or deodorant composition may further comprise other optional ingredient(s). The compositions can be in the form of a solid stick. The compositions may be free of dipropylene glycol, added water, castor wax, or any combination thereof. The antiperspirant composition may be anhydrous. The antiperspirant composition may be free of added water.

As consumers seek more natural ingredients in their antiperspirants and deodorants, one approach to formulation is to use emollients derived from natural oils. Emollients derived from natural oils are derived from plant sources, such as palm oil or coconut oil. One example of an emollient derived from natural oils may be a liquid triglyceride, defined as a triglyceride that is liquid at <NUM>. Thus, products that hope to emphasize natural ingredients may have a significant amount of a liquid triglyceride, for example. Derived directly from plant sources, liquid triglycerides are often short chains. Longer chain triglycerides may be used as structurants in deodorant or antiperspirant sticks, but the triglycerides of the present invention are liquid at room temperature (<NUM>) and tend to be shorter chains. The triglyceride used in the present application is caprylic / capric triglyceride.

Providing a deodorant stick having at least <NUM>% of a liquid triglyceride and structurants that have a melting point greater than <NUM> can result in a deodorant stick with a hardness from <NUM> (<NUM>*<NUM>) to <NUM> (<NUM>*<NUM>). Such a deodorant stick is able to comprise consumer-perceived natural ingredients, while offering a pleasant consumer experience in terms of its hardness.

In general, the greater amount of liquid in the formulation, the softer the deodorant stick may be. The more solids in the formulation leads to greater hardness. Because achieving a sufficient softness in a deodorant stick with natural ingredients can be a challenge, it can be beneficial to formulate with higher amounts of liquids such as liquid triglyceride.

Rather than using waxes or other high melting structurants, the deodorant stick comprise levels of liquid caprylic /capric triglyceride of at least <NUM>%, at least <NUM>% of the composition, or at least <NUM>% by weight of the composition. In some embodiments, the amount of liquid triglyceride may be from <NUM>% to <NUM>%, from <NUM>% to <NUM>%, from <NUM>% to <NUM>%, or from <NUM>% to <NUM>%, by weight, of the composition. The level of liquid triglyceride as referred to herein is the sum total of one or more types of liquid triglyceride in a particular deodorant stick.

The deodorant compositions of the present invention has a product or stick hardness from <NUM> (<NUM>*<NUM>) to <NUM> (<NUM>*<NUM>), as measured by penetration with ASTM D-<NUM> needle (see Hardness test method below). In some embodiments, the product hardness may be from <NUM> to <NUM> (from <NUM> to <NUM>*<NUM>), or from <NUM> to <NUM> (from <NUM> to <NUM>*<NUM>), from <NUM> to <NUM> (from <NUM> to <NUM>*<NUM>), or from <NUM> to <NUM> (from <NUM> to <NUM>*<NUM>.

The antiperspirant and deodorant compositions of the present invention comprise a suitable concentration of a primary as defined in the claims to help provide the compositions with the desired viscosity, rheology, texture and/or product hardness, or to otherwise help suspend any dispersed solids or liquids within the composition. A primary structurant may be the structurant that appears in the product in the highest amount (liquid triglycerides are not considered a structurant in this context). In some embodiments, the primary structurant may have a melting point of at least <NUM>, or from <NUM> to <NUM>, or from <NUM> to <NUM>, or from <NUM> to <NUM>.

The term "solid structurant" as used herein means any material known or otherwise effective in providing suspending, gelling, viscosifying, solidifying, and/or thickening properties to the composition or which otherwise provide structure to the final product form. These solid structurants include gelling agents, and polymeric or non-polymeric or inorganic thickening or viscosifying agents. Such materials will typically be solids under ambient conditions and include organic solids, crystalline or other gellants, inorganic particulates such as clays or silicas, or combinations thereof.

The concentration and type of solid structurant selected for use in the antiperspirant and deodorant compositions will vary depending upon the desired product hardness, rheology, and/or other related product characteristics. For most structurants suitable for use herein, the total structurant concentration ranges from <NUM>% to <NUM>%, more typically from <NUM>% to <NUM>%, or from <NUM>% to <NUM>%, by weight of the composition.

The structurant used in the present application is ozokerite.

The deodorant stick may further comprise one or more structural elements selected from the group consisting of waxes, natural oils, coconut oil, fractionated coconut oil, jojoba seed oil, olive oil, soybean oil, sunflower oil, and combinations thereof.

Other non-limiting examples of primary structurants suitable for use herein are described in <CIT>) and <CIT>).

The antiperspirant or deodorant composition can further comprise one or more of an additional, or secondary, structurant. The additional structurant may be present in an amount from <NUM> % to <NUM> %, by weight of the composition. The additional structurant(s) will be present at an amount less than the primary structurant.

Non-limiting examples of suitable additional structurants include stearyl alcohol and other fatty alcohols; hydrogenated castor wax (e.g., Castorwax MP80, Castor Wax, etc.); hydrocarbon waxes include paraffin wax, beeswax, carnauba, candelilla, spermaceti wax, ozokerite, ceresin, baysberry, synthetic waxes such as Fisher-Tropsch waxes, and microcrystalline wax; polyethylenes with molecular weight of <NUM> to <NUM> daltons; and solid triglycerides; behenyl alcohol, or combinations thereof.

Other non-limiting examples of additional structurants suitable for use herein are described in <CIT>) and <CIT>).

The antiperspirant stick compositions of the present invention can comprise a particulate antiperspirant active suitable for application to human skin. The concentration of antiperspirant active in the composition should be sufficient to provide the desired perspiration wetness and odor control from the antiperspirant stick formulation selected.

The antiperspirant stick compositions of the present invention comprise an antiperspirant active at concentrations of from <NUM>% to <NUM>%, and more specifically from <NUM>% to <NUM>%, by weight of the composition. These weight percentages are calculated on an anhydrous metal salt basis exclusive of water and any complexing agents such as, for example, glycine, and glycine salts. The antiperspirant active as formulated in the composition can be in the form of dispersed particulate solids having an average particle size or equivalent diameter of less than <NUM> microns, more specifically less than <NUM> microns, and even more specifically less than <NUM> microns.

The antiperspirant active for use in the anhydrous antiperspirant compositions of the present invention may include any compound, composition or other material having antiperspirant activity. More specifically, the antiperspirant actives may include any of the antimicrobial discussed above, or may also include astringent metallic salts, especially inorganic and organic salts of aluminum, zirconium and zinc, as well as mixtures thereof. Even more specifically, the antiperspirant actives may include aluminum-containing and/or zirconium-containing salts or materials, such as, for example, aluminum halides, aluminum chlorohydrate, aluminum hydroxyhalides, zirconyl oxyhalides, zirconyl hydroxyhalides, and mixtures thereof.

Aluminum salts for use in the anhydrous antiperspirant stick compositions include those that conform to the formula:.

More specifically, aluminum chlorohydroxides referred to as "<NUM>/<NUM> basic chlorohydroxide" may be used, wherein a=<NUM>, and "<NUM>/<NUM> basic chlorohydroxide", wherein a=<NUM>.

Processes for preparing aluminum salts are disclosed in <CIT>, Gilman, issued Jun. <NUM>, <NUM>; <CIT>, Jones et al. , issued Sep. <NUM>, <NUM>; <CIT>, Gosling et al. , issued Nov. <NUM>, <NUM>; and <CIT>, Fitzgerald et al. , published Dec. <NUM>, <NUM>.

Mixtures of aluminum salts are described in <CIT>, Shin et al. , published Feb. <NUM>, <NUM>.

Zirconium salts for use in the anhydrous antiperspirant stick compositions include those which conform to the formula:.

These zirconium salts are described in <CIT>. Zirconium salts that additionally contain aluminum and glycine, commonly known as "ZAG complexes," are believed to be especially beneficial. These ZAG complexes contain aluminum chlorohydroxide and zirconyl hydroxy chloride conforming to the above-described formulas. Such ZAG complexes are described in <CIT>; Great <CIT>; and <CIT>.

Also suitable for use herein are enhanced efficacy aluminum-zirconium chlorohydrex-amino acid which typically has the empirical formula AlnZr(OH)[3n+<NUM>-m(n+<NUM>)](Cl)[m(n+<NUM>)]-AAq where n is <NUM> to <NUM>, preferably <NUM> to <NUM>; m is <NUM> to <NUM> (which corresponds to M:Cl approximately equal to <NUM>-<NUM>), preferably <NUM> to <NUM> (which corresponds to M:Cl approximately equal to <NUM>-<NUM>); q is <NUM> to <NUM>, preferably <NUM> to <NUM>; and AA is an amino acid such as glycine, alanine, valine, serine, leucine, isoleucine, β-alanine, cysteine, β-amino-n-butyric acid, or γ-amino-n-butyric acid, preferably glycine. These salts also generally have some water of hydration associated with them, typically on the order of <NUM> to <NUM> moles per mole of salt (typically, <NUM>% to <NUM>%, more typically <NUM>% to <NUM>% by weight). These salts are generally referred to as aluminum-zirconium trichlorohydrex or tetrachlorohydrex when the Al:Zr ratio is between <NUM> and <NUM> and as aluminum-zirconium pentachlorohydrex or octachlorohydrex when the Al:Zr ratio is between <NUM> and <NUM>. The term "aluminum-zirconium chlorohydrex" is intended to embrace all of these forms. The preferred aluminum-zirconium salt is aluminum-zirconium chlorohydrex-glycine. Additional examples of suitable high efficacy antiperspirant actives can include Aluminum Zirconium Pentachlorohydrex Glycine, Aluminum Zirconium Octachlorohydrex Glycine, or a combination thereof. These high efficacy actives are more fully described in U.

Perfumes or fragrances are often a combination of many raw materials, known as perfume raw materials. Any perfume or fragrance suitable for use in an antiperspirant or deodorant composition may be used herein, including, but not limited to, natural or essential oils. In some embodiments, the composition may be free of, or substantially free of a synthetic fragrance. A synthetic fragrance is one mostly derived through chemical synthesis where the starting material is no longer intact, but is converted to the new fragrance chemical. In some embodiments, the deodorant or antiperspirant may comprise a fragrance composition comprising at least <NUM>% of natural oils, essential oils, or a combination thereof.

A natural or essential oil fragrance is a result of natural sources wherein the fragrance material is not altered (chemically modified) but extracted from its natural source. These sources can include, but are not limited to, bark, flowers, blossoms, fruits, leaves, resins, roots, bulbs, and seeds. Natural or essential oils go through an extraction process instead of chemical synthesis. Extraction processes include, but are not limited to, maceration, solvent extraction, distillation, expression of a fruit peel, or effleurage.

As discussed, an effective and consumer-preferred emollient may be a liquid triglyceride. In some embodiments, additional emollients may be used, such as plant oils (generally used at less than <NUM>%) including olive oil, coconut oil, sunflower seed oil, jojoba seed oil, avocado oil, canola oil, and corn oil. Additional emollients including mineral oil; shea butter; PPG-<NUM> butyl ether; isopropyl myristate; petrolatum; butyl stearate; cetyl octanoate; butyl myristate; myristyl myristate; C12-<NUM> alkylbenzoate (e.g., Finsolv. ); octyldodecanol; isostearyl isostearate; octododecyl benzoate; isostearyl lactate; isostearyl palmitate; isobutyl stearate; dimethicone, and any mixtures thereof.

The antiperspirant and deodorant compositions of the present invention may have a liquid triglyceride or natural oils as a solvent.

Also, non-volatile organic fluids may be present, for example, in an amount of <NUM>% or less, by weight of the composition.

Non-limiting examples of nonvolatile organic fluids include mineral oil, PPG-<NUM> butyl ether, isopropyl myristate, petrolatum, butyl stearate, cetyl octanoate, butyl myristate, myristyl myristate, C12-<NUM> alkylbenzoate (e.g., Finsolv. ), octyldodecanol, isostearyl isostearate, octododecyl benzoate, isostearyl lactate, isostearyl palmitate, and isobutyl stearate.

The anhydrous compositions of the present invention may further comprise any optional material that is known for use in antiperspirant and deodorant compositions or other personal care products, or which is otherwise suitable for topical application to human skin.

One example of an optional ingredient is a scent expression material. Scent expression or release technology may be employed with some or all of the fragrance materials to define a desired scent expression prior to use and during use of the products. Such scent expression or release technology can include cyclodextrin complexing material, like beta cyclodextrin. Other materials, such as, for example, starch-based matrices or microcapsules may be employed to "hold" fragrance materials prior to exposure to bodily-secretions (e.g., perspiration). The encapsulating material may have release mechanisms other than via a solvent; for example, the encapsulating material may be frangible, and as such, rupture or fracture with applied shear and/or normal forces encountered during application and while wearing. A microcapsule may be made from many materials, one example is polyacrylates.

Another example of optional materials are clay mineral powders such as talc, mica, sericite, silica, magnesium silicate, synthetic fluorphlogopite, calcium silicate, aluminum silicate, bentonite and montomorillonite; pearl pigments such as alumina, barium sulfate, calcium secondary phosphate, calcium carbonate, titanium oxide, finely divided titanium oxide, zirconium oxide, zinc oxide, hydroxy apatite, iron oxide, iron titrate, ultramarine blue, Prussian blue, chromium oxide, chromium hydroxide, cobalt oxide, cobalt titanate, titanium oxide coated mica; organic powders such as polyester, polyethylene, polystyrene, methyl methacrylate resin, cellulose, <NUM>-nylon, <NUM>-nylon, styrene-acrylic acid copolymers, poly propylene, vinyl chloride polymer, tetrafluoroethylene polymer, boron nitride, fish scale guanine, laked tar color dyes, laked natural color dyes; and combinations thereof.

Talc, if used at higher levels can produce a significant amount of white residue which has been found to be a consumer negative for product acceptance. Therefore it is best to limit the composition to less than <NUM>%, less than <NUM>%, less than <NUM>%, or less than <NUM>%, by weight of the composition.

Nonlimiting examples of other optional materials include emulsifiers, distributing agents, antimicrobials, pharmaceutical or other topical active, preservatives, surfactants, and so forth. Examples of such optional materials are described in <CIT>); <CIT>); and <CIT>).

The antiperspirant and deodorant stick products of the present invention may be made by mixing all the components of the products in an open-top or vented tank. Many powders come with bound moisture, especially naturally high moisture powders like starches. In a mostly anhydrous process with waxes, melting the waxes above their melt point can release this bound water as the batch temperature increases. In a closed tank process this water vapor will condense in the tank and drip back into the batch as water. This water can interact with the most water soluble ingredients in the batch to have negative effects on the product, including releasing the pH of any antimicrobial ingredient, which can then degrade any perfume ingredients in the batch. Additionally, the condensed water can interfere with the wax and produce a stick softer than intended.

The present invention reduces the risk of these negative consequences by minimizing the water solubility of the primary antimicrobial ingredients. The ideal process remedy for this behavior is to produce the batches in one of four ways:.

A method of making a deodorant composition or stick may comprise the steps of combining any of the herein described deodorant or antiperspirant composition components in an open tank system or a vented closed tank. The components may be mixed, heated, and then cooled into a stick product. In some embodiments, the deodorant components may comprise at least <NUM>% of a liquid triglyceride, by weight of the composition, and an antimicrobial in an open tank system, heating the components, mixing the components, and cooling the components.

The data in Table <NUM> above was generated with the following test method. The purpose of this assay is to determine if a compound or formulation has an antimicrobial effect in vitro.

It is understood that when not specifically noted in this procedure:.

Apparatus
Incubator at <NUM>; <NUM>-200ul <NUM> channel pipette; <NUM>-50ul <NUM> channel pipette; 1250ul <NUM> channel Thermo Scientific Matrix pipette; <NUM> well plate shaker (located in incubator); Beckman Coulter deep well cap mat #<NUM>; Beckman Coulter deep <NUM> well plates #<NUM>; Falcon <NUM> well tissue culture plates #<NUM>; Vortexer ; Culture tubes/caps Disposable sterile gloves; Sterile petri dishes; Standard microbiological lab equipment (sterile pipettes, syringes, tips, loops, etc.); Glass bottles/flasks for media; Autoclave; Parafilm; Spectrophotometer.

Inoculum Preparation
Prior to testing streak organisms for isolation on BHI with <NUM>% Tween <NUM> plates, wrap with parafilm and place in <NUM>OC incubator. When isolated colonies appear remove one representative colony from each plate and place each in <NUM> of BHI with <NUM>% Tween <NUM> media. Incubate at <NUM>OC with shaking overnight. Inoculate <NUM> BHI with <NUM>% Tween <NUM> (per <NUM> deep well plate to be tested) with 20ul of the overnight culture (<NUM>-<NUM> dilution). Master Plate Preparation
Compounds/formulations to be tested are diluted across a <NUM> deep well plate as shown below (for a <NUM>% stock solution). 800ul of <NUM>% saline is added to wells A1 and B1 (as these will be the negative and positive control respectively). 800ul each <NUM>% stock solution + positive control are added to wells C1 through H1. 400ul <NUM>% saline are added to all other wells. 400ul is then removed from #<NUM> well added to the #<NUM> well and mixed. This is then continued across the plate resulting in a <NUM>% dilution between wells across the plate (this can be easily accomplished with an automatic <NUM> channel Matrix pipette set to withdraw, dispense and mix).

In row A of a <NUM> deep well plate pipette 180ul of sterile BHI with <NUM>% Tween <NUM> as a negative growth control. All other wells receive 180ul of inoculum. From the master plate introduce 20ul to the corresponding row in the test plate using an <NUM>-channel pipette. Loaded plates are placed on a plate shaker in the <NUM>OC incubator and incubated overnight. The next day read the O. <NUM> on a plate reader. The MIC is the last well from the right that has no bacterial growth.

The penetration test is a physical test method that provides a measure of the firmness of waxy solids and extremely thick creams and pastes with penetration values not greater than <NUM> when using a needle for D1321. The method is based on the American Society for Testing and Materials Methods D-<NUM>, D1321 and D217 and DIN <NUM><NUM> and is suitable for all solid antiperspirant and deodorant products.

A needle or polished cone of precisely specified dimensions and weight is mounted on the bottom of a vertical rod in the test apparatus. The sample is prepared as specified in the method and positioned under the rod. The apparatus is adjusted so that the point of the needle or cone is just touching the top surface of the sample. Consistent positioning of the rod is critical to the measured penetration value. The rod is then released and allowed to travel downward, driven only by the weight of the needle (or cone) and the rod. Penetration is the tenths of a millimeter travelled following release.

General Instructions - All Penetrometers - Keep the instrument and needles/probes clean at all times, free from dust and grime. When not in use, store needles in a suitable container to avoid damage. Periodic calibration should confirm:.

Ensure the total weight of the shaft and needle is <NUM> ± <NUM> grams when the shaft is in free fall. Note: for modern, automated or digital systems this may be performed automatically and confirmed through annual calibration.

Claim 1:
A deodorant stick comprising:
a. at least <NUM>% by weight liquid triglyceride, wherein the triglyceride is liquid at <NUM>, wherein the liquid triglyceride is caprylic/capric triglyceride, wherein the total amount of liquid triglyceride is at least <NUM>% by weight;
b. a primary antimicrobial having a water solubility of at most <NUM>/L at <NUM>;
c. a fragrance composition comprising at least <NUM>% by weight of natural oils, essential oils, or a combination thereof; and
d. a primary structurant with a melting point of at least <NUM>, wherein the primary structurant is ozokerite;
said deodorant stick being free of an aluminum salt; and
said deodorant stick having a hardness from <NUM> (<NUM>*<NUM>) to <NUM> (<NUM>*<NUM>), as measured by penetration with ASTM D-<NUM> needle.