Patent Grant
12138332
This invention relates to the field of whipped or whippable formulations. More specifically, the invention relates to whipped or whippable formulations, such as for topical application, such as, for example, skincare products.
High viscosity and high solids products are often found to be difficult to distribute on the skin or a secondary surface and selection of an appropriate amount of product can often be difficult for a user to estimate.
Also, a key factor for ensuring the effectiveness of a formulation, such as skincare (such as, for example, diaper rash products), sunscreen, vitamins for oral administration, woundcare for animals or humans, whip cream, haircare, medical hair & scalp treatments, topical analgesics, skin protection, etc. is end-user compliance and satisfaction.
Ideally, the skincare formulation should be easily applied to the skin of the user, and have a good texture and “feel” on the skin of the users.
Likewise, other products, such as for suncare, vitamins for oral administration, woundcare for animals or humans, whip cream, for haircare, for medical hair & scalp treatments, for topical analgesics, for skin protection, etc. could benefit from being administered as a whipped product, without the possibility of abuse.
This disclosure provides a formulation in a package, which may be pressurized. The formulation comprises one or more skincare active agents and is co-mingled (co-processed) with a whipping agent (e.g., a gas propellant; a first gas propellant) prior to being filled under pressure into the package. The first propellant is added in sufficient amounts to be dispersed in the formulation. In certain embodiments, the package maintains at least a minimal amount of pressure until substantially all the formulation in the package is expelled as a whipped formulation. In certain embodiments, the package maintains at least a minimal amount of pressure to maintain the whipping agent dispersed in the formulation. In certain embodiments, the package comprises a pressure generating and maintaining component. In certain embodiments, the component comprises one or more (second) gas and/or liquid propellants. In certain embodiments, the component is present in the package in sufficient amounts and pressure to expel the formulation as a whipped formulation upon application of external force on the formulation in the package. In certain embodiments, the amounts of the pressure generating and maintaining component are sufficient to expel substantially all the formulation in the package as a whipped formulation. In certain embodiments, the one or more gas and/or liquid propellants do not co-mingle with the formulation.
In other aspects, this disclosure provides a method of preparing a whippable formulation, comprising: filling a formulation comprising one or more skincare active agents co-mingled (co-processed) with a whipping agent (e.g., a gas propellant; a first gas propellant) under pressure into a package; wherein the whipping agent is added in sufficient amounts to be dispersed in the formulation. In certain embodiments, the package is under sufficient pressure suitable to maintain the whipping agent dispersed in the formulation. In certain embodiments, the pressurized package is under sufficient pressure to expel the formulation as a whipped formulation upon application of external force on the formulation in the package. In certain embodiment, the method is performed under controlled temperature. In certain embodiments, the package maintains at least a minimal amount of pressure until substantially all the formulation in the package is expelled as a whipped formulation. In certain embodiments, the package comprises a pressure generating and maintaining component. In certain embodiments, the component comprises one or more (second) gas and/or liquid propellants. In certain embodiments, the pressure generating and maintaining component is present in the package in sufficient amounts and pressure to expel the formulation as a whipped formulation upon application of external force on the formulation in the package. In certain embodiments, the one or more gas and/or liquid propellants do not co-mingle with the formulation.
In other aspects, this disclosure provides a method of using a formulation that is a whipped formulation product disclosed herein, comprising administering the formulation to a subject in need thereof.
In other aspects, this disclosure provides a package comprising the formulation disclosed herein.
Numerous other aspects are provided in accordance with these and other aspects of the invention. Other features and aspects of the present invention will become more fully apparent from the following detailed description and the appended claims.
As used herein, the word “a” or “plurality” before a noun represents one or more of the particular noun. For the terms “for example” and “such as,” and grammatical equivalences thereof, the phrase “and without limitation” is understood to follow unless explicitly stated otherwise. As used herein, the term “about” is meant to account for variations due to experimental error. All measurements reported herein are understood to be modified by the term “about,” whether or not the term is explicitly used, unless explicitly stated otherwise. As used herein, the singular forms “a,” “an,” and “the” include plural referents unless the context clearly dictates otherwise.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Methods and materials are described herein for use in the present invention; other, suitable methods and materials known in the art can also be used. The materials, methods, and examples are illustrative only and not intended to be limiting. All publications, patent applications, patents, sequences, database entries, and other references mentioned herein are incorporated by reference in their entirety. In case of conflict, the present specification, including definitions, will control.
This disclosure provides a formulation in a package, which may be pressurized. The formulation comprises one or more skincare active agents and is co-mingled (co-processed) with a whipping agent (e.g., a gas propellant; a first gas propellant) prior to being filled under pressure (and in certain embodiments under controlled temperature) into the package. The whipping agent is added in sufficient amounts to be dispersed in the formulation. In certain embodiments, the package maintains at least a minimal amount of pressure until substantially all the formulation in the package is expelled as a whipped formulation. In certain embodiments, the package maintains at least a minimal amount of pressure to maintain the whipping agent dispersed in the formulation. In certain embodiments, the package comprises a pressure generating and maintaining component. In certain embodiments, the component comprises one or more (second) gas and/or liquid propellants. In certain embodiments, the component is present in the package in sufficient amounts and pressure to expel the formulation as a whipped formulation upon application of external force on the formulation in the package. In certain embodiments, the amounts of the pressure generating and maintaining component are sufficient to expel substantially all the formulation in the package as a whipped formulation. In certain embodiments, the one or more as and/or liquid propellants do not co-mingle with the formulation. In certain embodiments, one of the one or more skincare active agents is a solid ingredient or a high viscosity ingredient. In certain embodiments, the formulation comprises less than 20% water.
No UV filter substances are used for the foam-boosting of self-foaming.
The disclosed whipped formulation may be referred to herein as whipped formulation, whipped formulation product, whipped product, and the like.
The disclosed whippable formulation may be referred to herein as whippable formulation, whippable formulation product, whippable product, and the like.
A whipped formulation is at one time a whippable formulation.
The term “can” may be used to also mean “package.”
A subject may be a human subject (user) or may be an animal subject (user). The terms “subject” and “user” are used interchangeably.
In other aspects, this disclosure provides a method of preparing a whippable formulation, comprising: filling a formulation comprising one or more skincare active agents co-mingled (co-processed) with a whipping agent (e.g., a gas propellant; a first gas propellant) under pressure into a package, which may be pressurized; wherein the whipping agent is added in sufficient amounts to be dispersed in the formulation. In certain embodiments, the package is under sufficient pressure suitable to maintain the whipping agent dispersed in the formulation. In certain embodiments, the package is under sufficient pressure to expel the formulation as a whipped formulation upon application of external force on the formulation in the package. In certain embodiments, the method is performed under controlled temperature. In certain embodiments, the package maintains at least a minimal amount of pressure until substantially all the formulation in the package is expelled as a whipped formulation. In certain embodiments, the package comprises a pressure generating and maintaining component. In certain embodiments, the component comprises one or more (second) gas and/or liquid propellants. In certain embodiments, the pressure generating and maintaining component is present in the package in sufficient amounts and pressure to expel the formulation as a whipped formulation upon application of external force on the formulation in the package. In certain embodiments, the one or more gas and/or liquid propellants do not co-mingle with the formulation. In certain embodiments, one of the one or more skincare active agents is a solid ingredient or a high viscosity ingredient. In certain embodiments, the formulation comprises less than 20% water.
In other aspects, this disclosure provides a method of using a formulation that is a whipped formulation product disclosed herein, comprising administering the formulation to a subject in need thereof.
In other aspects, this disclosure provides a package, which may be pressurized, comprising a whippable formulation. The formulation comprises one or more skincare active agents and is co-mingled (co-processed) with a whipping agent (e.g., a gas propellant; a first gas propellant) prior to being filled under pressure (and in certain embodiments under controlled temperature) into the package. In certain embodiments, the package maintains at least a minimal amount of pressure until substantially all the formulation in the package is expelled as a whipped formulation. In certain embodiments, the package maintains at least a minimal amount of pressure to maintain the whipping agent dispersed in the formulation. In certain embodiments, the package comprises a pressure generating and maintaining component. In certain embodiments, the component is present in the package in sufficient amounts and pressure to expel the formulation as a whipped formulation upon application of external force on the formulation in the package. In certain embodiments, the amounts of the pressure generating and maintaining component are sufficient to expel substantially all the formulation in the package as a whipped formulation. In certain embodiments, the pressure generating and maintaining component comprises one or more (second) gas and/or liquid propellants. In certain embodiments, the one or more gas and/or liquid propellants do not co-mingle with the formulation. In certain embodiments, one of the one or more skincare active agents is a solid ingredient or a high viscosity ingredient. In certain embodiments, the formulation comprises less than 20% water.
In certain embodiments, the whipped formulation comprises a high concentration of a solid ingredient (i.e., high solids), a high viscosity ingredient, or both.
In certain embodiments, a solid ingredient is one that is not easily dissolved in water or another solvent. In certain embodiments, the solid ingredient includes, without limitation, zinc oxide, titanium dioxide, wax, inorganic clay, minerals, microcapsules and other solid particles, or a mixture thereof. In certain embodiments, the formulation comprises from about 10% to about 85% solids content (i.e., solid ingredient being from about 10% to about 85%). In certain embodiments, the formulation comprises from about 10% to about 60% solids content. In certain embodiments, the formulation comprises from about 10% to about 50% solids content. In certain embodiment, the solid ingredient may be up to and in excess of about 40%. In certain embodiments, the formulation comprises zinc oxide, such that the high solids content is up to or in excess of about 40%, about 50%, about 60%, about 85% etc.
In certain embodiments, a high viscosity ingredient has a viscosity of about 75,000-450,000 cps.
The whipped formulation comprising high solids or high viscosity ingredients may be a topical therapeutic skin care formulation. This formulation provides easily “spreadable”, low drag application experience, with such an experience being highly desirable for the treatment of sensitive or damaged skin. Such formulation generally has a specific gravity in excess of 1. For example, the specific gravities may be about, or in excess of, 1.1-3; such as, for example, about 1.1, or about 1.4-1.5. These formulations can be improved through infusion of compressed gas, which in turn is held in a steady gas-infused super saturated state, until time of release into ambient conditions, at which time the formulation becomes “transformed” into a reduced density product form, through the expansion of highly compressed saturated gas.
The whipped formulation comprising high solids or high viscosity ingredients is effectively transformed from a paste into a reduced density gas emulsion with a multitude of gas microbubbles. These bubbles are continuously distributed through the whipped formulation and may express on the surface of the dispensed product as agglomerated bubbles, signaling to the consumer the uniqueness of the transformed formulation, further differentiating it from standard BOV dispensed products and further reinforcing the perception of a “light and airy” application experience. The density of the formulation may be reduced, lowering “pre-gas” or “cut-bag” pressures thus reducing finished can pressures (of the package) and may allow for lower pressurized can ratings to be leveraged, further reducing costs and technical requirements of the package. Certain first gas propellants, includes, without limitation, oxygen and carbon dioxide, may also be used to evoke various therapeutic and/or cosmetic skin care responses.
This transformed formulation also enables the use of “soft touch” secondary application tools, including, without limitation, sponges, brushes, and the like, further increasing the utility of the formulation by allowing the user to apply what would normally be a thick, viscous paste in a fashion more akin to a lower viscosity, lower drag cream in a “no touch” manner.
An additional benefit of this system is the described reduced viscosity transformation of the high solids formulation may help the user to better visually control the amount of product applied, while still permitting the creation of a highly occlusive coating. This is achieved as a result of the increased volume to mass product ratio created during dispensing.
In certain embodiments, the pressurized package is under sufficient pressure to expel the formulation upon application of external force on the formulation, either with a second gas and/or liquid propellant or mechanical force to generate enough pressure to keep the first gas microdispersed or in emulsion.
In certain embodiments, the disclosed formulations and methods allow for very high levels of inert gas dissolved into the product and effectively held under pressure in a gas-emulsion, preventing unwanted bubble agglomeration, providing for highly uniform product characteristics. The result is a rich, thick “whipped-cream-style” lotion that provides confidence of sunscreen coverage (in the case where the product is a sunscreen), while offering surprisingly fast “rub-in”; while not altering the inherent moisturization and protection properties of the otherwise thick, lipid-rich base formulation.
Whippable products include, in addition to for skincare and suncare (sunscreen and after sun care), for example and without limitation:
Category—Class—Whipped Benefit
Thus, in certain embodiments, the formulation disclosed herein comprise one or more active agents for each of the above formulations.
In certain embodiments, the whipped formulation product is a skincare product, comprising one or more skincare active agents. In certain embodiments, the whipped formulation is a diaper rash product.
In certain embodiments, the whipped formulation comprises high solids (including zinc oxide), up to and in excess of about 85%.
A subject may be a human subject (user) or may be an animal subject (user). “Subject” and “user” are used interchangeably.
In certain embodiments, the formulation further comprises a foaming agent. In certain embodiments, the formulation is for topical application.
In certain embodiments, the pressurized package in which pressure may be generated and/or maintained sufficient for the disclosed formulations is a Bag-on-valve, Piston Can, or Bag-in-Can. In other embodiments, the pressurized package is a mechanical pressure system, including for example, bladder system (such as Exxal Atomos System), which is a PowerContainer system with a rubber bladder around the outside providing pressure to the internal volume.
In certain embodiments, the package is a bag on valve (BOV) pressurized assembly, comprising a two way fill/dispensing valve, an attached internal high barrier bag affixed to said valve, and rigid container capable of holding positive pressure, affixed to the valve. In certain further embodiments, the container is glass, barrier resin, metal/alloy, or another material capable of holding positive pressure. In certain other further embodiments, the container is pre-pressurized with one or more gas and/or liquid propellants prior to filling. In certain further embodiments, the BOV pressurized assembly dispenses the whipped product in a metered dispensing system and not a continuously dosing system.
In certain embodiments, pre-pressurizing the package is not needed. In certain embodiments, the package is under Zero Cut Bag Pressure, where gas is present around bag but not pressurized above ambient. Filling the package at ambient pressure, the pressure inside the package would increase as the BOV expands. In certain embodiments, the package comprises an elastomeric tube/bag (akin to a tied off surgical tube). In certain further embodiments, a slight vacuum is applied. In certain embodiments, the package is pressure agnostic, in which the container cannot hold pressure around the bag. In certain embodiments, the package has Negative Cut Bag Pressure, where vacuum is present around the bag but not pressurized above ambient. Other such systems may be used, such as the Sterilflo® system (https://www.hydrasense.ca/en/why-choose-hydrasense/steriflo/).
In certain embodiments, the pressurized package can comprise a “pressure generating and maintaining component,” which may be a component that generates and/or maintains pressure in the package. It may refer to a chemical component or components which generate pressure, e.g., compressed gas, while inside an enclosed package, device or container (such as a can, for example). Non-limiting examples of such pressure generating and maintaining components are compressed gases/propellants and liquid propellants such as, for example, CO2, propane, butane, isobutane, dimethyl ether, nitrous oxide, nitrogen, oxygen, air, isopentane, hydrofluroolefin, and the like, and suitable blends of such propellants. When a valve is opened by applying an external force, the formulation or ingredients in the device are dispensed in a ‘whipped’ form or a foamy form. This chemical component or components does not co-mingle with the formulation and may not be dispended with the whipped formulation.
A “skincare active agent” includes all those materials which are regarded as acceptable for use as active skin-protecting/treating ingredients. A skincare active agent includes, for example and without limitation, skin protectants, anti-inflammatory agents, antioxidants, topical anesthetics, antimycotics, keratolytics, and/or anti-aging agents. Approval by a regulatory agency may sometimes be required for inclusion of active agents in formulations intended for human contact including but not limited to zinc oxide for diaper rash treatments or petrolatum, white petrolatum, mineral oil, glycerin and dimethicone as skin protectants, ibuprofen, diclofenac, felbianc, ketoprofen, or piroxicam, as topical anti-inflammatories, lidocaine and its salt forms, and benzocaine and its salt forms as topical anesthetics, Imidazole, triazole, and triazole antifungals (e.g., miconazole, clotrimazole, efinaconazole, and abafungin), terbinafine hydrochloride, tolnaftate as antimycotics, salicylic acid, urea, and lactic acid as keratolytics as well as agents used as self-tanners or sunscreen active ingredients and the like.
Other active agents are contemplated. These include, for example and without limitation, sunscreen active agents, after sun active agents, vitamins, food, etc. Any active agents that can be included as a whipped formulation or a whippable formulation are within the scope of this invention.
In certain embodiments, the package does not display any bearding. Bearding is leakage forced by continued expansion of product still contained within the flow channel of the actuator.
In certain embodiments, the formulation is characterized by microdispersion. In certain embodiments, the formulation is characterized by substantially consistent microvoid after the formulation is expelled from the package. In certain embodiments, the formulation is highly emollient after the formulation is expelled from the package. In certain embodiments, the formulation is readily spreadable and spread evenly after the formulation is expelled from the package.
In certain embodiments, the whipping agent is an aerosol propellant (including hydrocarbon propellant, compressed gas propellant, soluble gas propellant, and liquefied gas propellant) or a liquid propellant.
In certain embodiments, the whipping agent is a gas propellant. The gas propellant is, for example and without limitation, nitrogen, nitrous oxide, carbon dioxide, Argon, air or oxygen. In certain embodiments, the gas propellant in the formulation is between about 0.01% w/w to about 15.00% w/w.
In certain embodiments, the whipping agent is a liquefied gas propellant, which includes, for example and without limitation, propane, isobutene, N-butane, Dymel 152a, 134a, hydrocarbons, DME (dimethyl ether), 1,3,3,3-tetrafluoropropene, and HFCs (1,1,1,2-tetrafluoroethane).
In certain embodiments, the whipping agent is a hydrocarbon propellant, which includes, for example and without limitation, methane, ethane, propane, butanes, and pentanes.
In certain embodiments, the formulation has one or more of characteristics such as little or no wetness after application, having a collapse time of at least 60 seconds, or structurally stable for at least 10 minutes.
The disclosed whipped formulation product represents the careful culmination of advancements in formulation, processing, and packaging to meet the end result of delivering a rich, creamy, spreadable, lightweight whipped product for consumer application.
Formulation:
Non-shear thickening emulsion chemistry has been developed to allow for high levels of gas dispersion, physical stability during temperature and pressure extremes, and post-dispensing foam stability. The chemistry has also been customized to allow for the inclusion of consumer-relevant ingredients that may include, for example and without limitation, skincare active agents (e.g., diaper rash treatment agents), skin protectants, moisturizers, emulsifying agents, film forming agents, thickening agents, skin feel aesthetic enhancers, antifungals, pH adjusters, pro vitamin additives, physical skin barriers, anti-bacterial agents, skin colorants, etc. Other ingredients are also contemplated, such as, without limitation, pain relief additives.
Processing:
In processing of certain embodiments, the blended formulation is transferred into a hopper, pressurized and under a controlled temperature, rate of flow and pressure, and is transferred into a high shear, continuous-flow, high-pressure “whipping” head, which rapidly mixes the base formulation with a series of infusion gas injector ports which controls the gas pressure and rates of flow with a selection of gases (or gas) to rapidly co-mingle the whipping agent and formulation solution, effectively dispersing the gas into the formulation prior to injection into the package. The gas-infused formulation is then tested for density inline and controlled under pressure and finally injected under pressure into the desired package.
In certain embodiments, the whipping agent is co-mingled with the formulation prior to filling the formulation into the package.
In certain embodiments, the whipping agent is nitrous oxide gas. In certain embodiments, the nitrous oxide in the formulation is about 0.1% w/w to about 4.0% w/w. In certain embodiments, the nitrous oxide in the formulation is about 0.1% w/w to about 10.0% w/w. In certain embodiments, the Nitrous Oxide in the formulation is about 0.1% w/w to about 1.9% w/w. In certain embodiments, the nitrous oxide in the formulation is about 0.1%, 1.0%, 1.9%, 2.0%, 3.0%, 4.0%, 5.0% w/w to about 6%, 7%, 8%, 9%, 10 w/w. Nitrous oxide has a slight sweet odor that can contribute to fragrance benefits (dual purpose gas benefits). Nitrous Oxide has a slight sweet odor that can contribute to fragrance benefits (dual purpose gas benefits).
In certain embodiments, certain other gases can serve as a particularly good whipping agent, as evaluated by the known or estimated Ostwald Coefficients of the blended mixture and gases. Taking into consideration the potential negative effects of co-mingling of the gases with base blended formulation, example being CO2, which can react with water-containing formulas to create carbonic acid and cause shifts in product pH. Alternatively, CO2 can be used as a whipping gas to deliberately modify the pH of the formulation to reach targeted pH levels. Gas propellant or combinations may also include, without limitation, CO2, isobutane, nitrogen, Argon, air, oxygen, isopentane, other suitable gases, and combination thereof.
In certain embodiments, the whipping agent in the formulation is between about 0.01% w/w to about 15.00% w/w.
Unless otherwise noted or otherwise clear in context to a person of ordinary skill in the art, all % herein are weight to weight (w/w).
Packaging:
In certain embodiments, the pressure in the pressurized package is initially between about 15 psig to about 60 psig. In certain embodiments, the final pressure in the pressurized package is between about 80 psig to about 160 psig. In certain embodiments, the pressure initially is about 40 psig to 45 psig. In certain embodiments, the final pressure is about 110 psig to 120 psig.
In certain embodiments, the package is a Bag on Valve (BOV) pressurized assembly, comprising a two way fill/dispensing valve, an attached internal high barrier bag (affixed to valve), and rigid container capable of holding positive pressure (affixed to the valve). The container may be glass, barrier resin, metal/alloy, or another material capable of holding positive pressure. The container may be “pre-pressurized” with a combination of gaseous and/or liquid propellants prior to filling, with internal pressure expected to build as the internal volume is displaced during pressurized BOV filling.
The Bag on Valve assembly and accompanying “air gap” created between bag and the pressurized rigid container help to create an insulated barrier between the formulation and the user environment. This isolative barrier is helpful to moderate the temperature swings that might be experienced when taking this product from an ambient (indoor) location to a cooler or warmer environment, such as into the sun or into vehicles located in low/high temperature environments. This barrier helps to buffer formulation temperature change and help the formulation deliver a more consistent product experience (lower temperatures can form more rigid foam structures and high temperatures can cause weaker foam structures). This feature can be particularly useful for products formulated with lower melt point foam-formers, intended for use in elevated temperature environments.
Bag on Valve delivery systems differ from traditional aerosol delivery systems in at least the following district ways: Aerosols require propellant gases to be co-joined or co-mingled into the base formulation, as would be the case in single or multiphase system. These systems use the propellant gas to both expel the product and as a foaming and/or particle breakup agent. By contrast, a Bag on Valve system includes the use of a bag within a pressurized package. The bag is in direct contact with the single phase formulation and is expelled by application of pressure to the outside of the bag. As such, the propellant gas inside the package never comes in contact with the product. Particle breakup or foaming can be accomplished through the dispensing actuator design and/or through the inclusion of a secondary gas within the formulation.
This BOV design has several distinct benefits over traditional aerosol systems including without limitation:
For example, in certain embodiments, Nitrous Oxide is used as a whipping agent without allowing “free gas” to be expelled and potentially abused. By contrast, whipped cream packaging which is sold in a traditional aerosol permits the user the ability to release and potentially abuse the gas propellant/whipping agent.
The pressure generating and maintaining component may be a gas, such as gaseous propellant, a liquid, such as a liquid propellant or a blend of gas and liquid. As used herein, a gaseous propellant may also be a compressed gas, such as CO2, nitrous oxide and the like. As used herein, a liquid propellant may also be a liquefied gas, such as isobutane and the like.
The pressure generating and maintaining component can be formulated inside the device in a variety of ways, depending upon the nature of the component or components that form the pressure generating and maintaining component. The vehicle, while acting as pressure-generator, may be a gas, even though it may have been packaged as, for example, a gas, a liquid or a solid. Non-limiting examples of the gas are carbon dioxide (CO2), nitrous oxide (N2O) and the like. Thus, for example, if the vehicle is carbon dioxide, the carbon dioxide can be ‘derived’ inside the sealed pressurized container in several ways. For example, the gas could be pumped into the container.
If generating the gas by chemical reaction between a base and an acid, non-limiting examples of suitable bases include sodium bicarbonate, sodium carbonate, potassium bicarbonate, potassium carbonate and the like. Non-limiting examples of suitable acids include acetic acid, citric acid and the like. Sodium bicarbonate with citric acid is a suitable combination. Because the components are being combined inside of the sealed container (device), the gas produced during the reaction is trapped which pressurizes the container.
One advantage of the inventive system is that the gas introduced or produced may be non-flammable.
In certain embodiments, the whipped formulation product is characterized by microdispersion. In certain embodiments, the whipped formulation product is characterized by substantially consistent microvoid.
In certain embodiments, the whipping agent is a suitable gas. In certain embodiments, the whipping agent is co-mingled with the formulation prior to filling the formulation into the package.
In certain embodiments, the whipping agent is nitrous oxide gas. In certain embodiments, the nitrous oxide in the formulation is about 0.1% w/w to about 4.0% w/w. In certain embodiments, the nitrous oxide in the formulation is about 0.1% w/w to about 10.0% w/w. In certain embodiments, the Nitrous Oxide in the formulation is about 0.1% w/w to about 1.9% w/w. In certain embodiments, the nitrous oxide in the formulation is about 0.1%, 1.0%, 1.9%, 2.0%, 3.0%, 4.0%, 5.0% w/w to about 6%, 7%, 8%, 9%, 10 w/w. Nitrous oxide has a slight sweet odor that can contribute to fragrance benefits (dual purpose gas benefits).
In certain embodiments, certain other gases can serve as a particularly good whipping agent, as evaluated by the known or estimated Ostwald Coefficients of the blended mixture and gases. Taking into consideration the potential negative effects of co-mingling of the gases with base blended formulation, example being CO2, which can react with water-containing formulas to create carbonic acid and cause shifts in product pH. Alternatively, CO2 can be used as a whipping gas to deliberately modify the pH of the formulation to reach targeted pH levels. Gas propellant or combinations include, without limitation, CO2, argon, isobutane, nitrogen, Argon, air, oxygen, isopentane, other suitable gases, and combination thereof.
In certain embodiments, the whipping agent in the formulation is between about 0.01% w/w to about 15.00% w/w.
In certain embodiments, the whipping agent is an aerosol propellant (including hydrocarbon propellant, compressed gas propellant, soluble gas propellant, and liquefied gas propellant) or a liquid propellant.
In certain embodiments, the whipping agent is a gas propellant. The gas propellant is, for example and without limitation, nitrogen, nitrous oxide, carbon dioxide, Argon, air or oxygen. In certain embodiments, the gas propellant in the formulation is between about 0.01% w/w to about 15.00% w/w.
In certain embodiments, the whipping agent is a liquefied gas propellant, which includes, for example and without limitation, propane, isobutene, N-butane, Dymel 152a, 134a, hydrocarbons, DME (dimethyl ether), 1,3,3,3-tetrafluoropropene, and HFCs (1,1,1,2-tetrafluoroethane).
In certain embodiments, the whipping agent is a hydrocarbon propellant, which includes, for example and without limitation, methane, ethane, propane, butanes, and pentanes.
In certain embodiments, the whipped formulation product comprises at least one recognized skincare active agent.
In certain embodiments, the whipped formulation product further comprises other ingredients, such as, for example and without limitation, one or more fatty alcohols—selected from, for example and without limitation, cetyl alcohol, stearyl alcohol, myristyl alcohol, hydroxystearyl alcohol, oleyl alcohol, isostearyl alcohol, lauryl alcohol, hexadecyl alcohol, ricinoleyl alcohol, behenyl alcohol (lanette 22), erucyl alcohol and 2-octyl-dodecanol. In certain embodiments, the whipped formulation is an After Sun lotion (contains Cetyl alcohol) but optionally without any added behenyl alcohol.
In certain embodiments, the physical stability of the whipped products obtained may also be characterized by means of these tests: determination of the organoleptic characteristics (e.g., aspect, color, odor), characterization of the texture (e.g., thick, fluid, greasy, non-greasy), and characterization of the spreadability.
In one embodiment, the disclosed whipped product formulation dispenses in a continuous stream when an external pressure is applied to the device, such as by depressing the valve/actuator, thereby eliminating the need to squeeze and shake the formulation out of a bottle or tube.
In another embodiment, the disclosed whipped product in its device (package) operates as a “one-touch” delivery system; in such system, the user will hold down the actuator until the desired amount of formulation is dispensed.
In another embodiment, the disclosed whipped product in its package offers a continuous delivery system for an application, such as, for example and without limitation, skincare applications and suncare applications. Traditionally, “continuous delivery” is typically offered as a spray product and has been very successful due to the ease and speed that it provides for sunscreen application. Many consumers, however, prefer lotions/gels over sprays and would benefit from a continuous delivery mechanism. The present invention offers such an advantage.
The disclosed whipped formulation product can be used for any application that would benefit from such product, including, for example and without limitation, skincare, sunscreen, after sun care, vitamins, woundcare, etc. For each application, the formulation needs to comprise the corresponding active agent(s) and may further comprise other appropriate ingredients.
The disclosed whipped product dispenses in a light whipped form, infused with tiny bubbles that make the texture of the formulation lighter, smoother and easier to spread across the skin. This texture also makes the formulation feel less greasy and more aesthetically pleasing on hands and skin, leaving a ‘sumptuous’ feel during application. This formulation spreads quickly as the user rubs the formulation into the skin. Such a formulation may even prevent excess application of the agent and may offer ecological advantages.
In another embodiment, the disclosed whipped product offers an easier, faster, smoother, and less greasy skincare formulation than a traditional formulation.
The term “emulsion” identifies oil-in-water (o/w) or water-in-oil (w/o) type dispersion formulations intended for application to the skin, and air emulsion. Such dispersion formulations include, for example and without limitation, lotions and creams providing cosmetic or therapeutic benefits. The emulsions may contain any of a number of desired “active” ingredients, including skin colorants, drug substances (such as anti-inflammatory agents, antibiotics, topical anesthetics, antimycotics, keratolytics, etc.), skin protectants or conditioners, humectants, ultraviolet radiation absorbers, food, vitamins, etc., depending on the intended uses for the formulations.
In certain embodiments, the whipped formulation product comprises one or more of a thickening agent and/or an emulsifying agent.
Suitable emulsifiers are those known in the art for producing oil-in-water type emulsions. An aqueous external phase is preferred by many people for skin contact, since it is not as likely to produce an oily or greasy sensation when it is being applied, as is an emulsion having an oil external phase. The typical oil-in-water emulsifier has a hydrophilic-lipophilic balance (frequently abbreviated as “HLB”) value greater than about 9, as is well known in the art; however, this “rule” is known to have numerous exceptions. The chosen emulsifier, depending upon its chemical nature, will be a component of either the oil or aqueous phase or both, and assists with both the formation and the maintenance, or stability, of the emulsion.
Non-limiting examples of suitable emulsifiers or surfactants include pharmaceutically acceptable, non-toxic, non-ionic, anionic and/or cationic surfactants. Examples of suitable non-ionic surfactants include, for example and without limitation, glycerol fatty acid esters such as glycerol monostearate, glycol fatty acid esters such as propylene glycol monostearate, polyhydric alcohol fatty acid esters such as polyethylene glycol (400) monooleate, polyoxyethylene fatty acid esters such as polyoxyethylene (40) stearate, polyoxyethylene fatty alcohol ethers such as polyoxyethylene (20) stearyl ether, polyoxyethylene sorbitan fatty acid esters such as polyoxyethylene sorbitan monostearate, sorbitan esters such as sorbitan monostearate, alkyl glycosides such as cetearyl glucoside, fatty acid ethanolamides and their derivatives such as the diethanolamide of stearic acid, Prolipid and the like. An example of a suitable Prolipid is Prolipid 141 which lists behenyl alcohol, glyceryl stearate, palmitic acid, stearic acid, myristyl alcohol, lauryl alcohol, cetyl alcohol and lecithin as its ingredients in its Formula Data Sheet. Examples of suitable anionic surfactants are soaps including, for example and without limitation, alkali soaps, such as sodium, potassium and ammonium salts of aliphatic carboxylic acids, usually fatty acids, such as sodium stearate. Organic amine soaps include, for example and without limitation, organic amine salts of aliphatic carboxylic acids, usually fatty acids, such as triethanolamine stearate. Metallic soaps include salts of polyvalent metals and aliphatic carboxylic acids, usually fatty acids, such as aluminum stearate. Other classes of suitable anionic surfactants include, for example and without limitation, sulfated fatty acid alcohols such as sodium lauryl sulfate, sulfated oils such as the sulfuric ester of ricinoleic acid disodium salt, and sulfonated compounds such as alkyl sultanates including sodium cetane sulfonate, amide sulfonates such as sodium N-methyl-N-oleyl laurate, sulfonated dibasic acid esters such as sodium dioctyl sulfosuccinate, alkyl aryl sulfonates such as sodium dodecylbenzene sulfonate, alkyl naphthalene sulfonates such a sodium isopropyl naphthalene sulfonate, petroleum sultanate such as aryl naphthalene with alkyl substitutes. Examples of suitable cationic surfactants include, for example and without limitation, amine salts such as octadecyl ammonium chloride, quaternary ammonium compounds such as benzalkonium chloride. Non-limiting examples of emulsifiers include a mixture of cetearyl glucoside and cetearyl alcohol, available under the trade name Emulgade PL68/50 from Henkel KGaA, and PEG 30 dipolyhydroxy stearate, available under the trade name Arlacel 135 from ICI. Also preferred are various C12-15, C12-16 and C14-15 alcohols available from various manufacturers, and Ceteareth 2, 10, 18, 22, Ceteth-1 and 20, cetyl dimethicone copolyol, and cetyl phosphate, glyceryl stearate, Oleth 3 and 10, polyglyceryl 3 methylglucose dis-tearate sorbitan isostearate, steareth 2, 10, and/or 20.
Other suitable emulsifiers are those known in the art for producing water-in-oil type emulsions. Non-limiting examples of some suitable water-in-oil emulsions include, for example and without limitation, Cithrol GMO 50-LQ (Glyceryl Oleate (&) Propylene Glycol), SIMALINE WO (PEG-30 Dipolyhydroxystearate; available from Seppic), FLUIDANOV 20X (Octyldodecanol & Octyldodecyl Xyloside; available from Seppic), ES-5300 (Lauryl PEG-10 Tris(trimethylsiloxy)silylethyl Dimethicone; available from Dow Corning), Abil EM90 (Cetyl PEG/PPG-10/1 Dimethicone; available from Evonik) and Abil WE09 (Polyglyceryl-4 Isostearate and Cetyl PEG/PPG-10/1 Dimethicone and Hexyl Laurate; available from Evonik). The typical water-in-oil emulsifier has a HLB value of about 4 to about 6, however, this “rule” is also known to have numerous exceptions.
It may be advantageous to incorporate thickening agents, such as, for instance, Avicel RC-591, Carbopol Ultrez, Carbopol ETD 2001, available from the B. F. Goodrich Co, Abil Wax 9801, a surfactant available from Evonik, Alginic Acid, available from Kelco, cellulose gum, available from TIC Gums, ammonium acrylates copolymer, ammonium polyacryloyl dimethyl taurate, bentonite available from Southern Clay, guar hydroxpropyltrimonium chloride available from Henkel, hydroxy propylprocellulose available from Aqualon, magnesium aluminum silicate, available from Salomon, potassium alginate available from Kelco, beeswax available from Strah & Pitsch, and behenyl alcohol available from Nikko.
The disclosed formulation/formulations may contain a wide range of additional, optional components. The CTFA Cosmetic Ingredient Handbook, Seventh Edition, 1997, the Eighth Edition, 2000, and the personal care council website (http://www.personalcarecouncil.org/) describe a wide variety of cosmetic and pharmaceutical ingredients commonly used in skin care formulations, which are suitable for use in the formulations of the present invention. Examples of these functional classes disclosed in these references include, for example and without limitation: absorbents, abrasives, anticaking agents, anti-foaming agents, antioxidants, binders, biological additives, buffering agents, bulking agents, chelating agents, chemical additives, colorants, cosmetic astringents, cosmetic biocides, cryoprotectants, film stabilizers, denaturants, drug astringents, external analgesics, film formers, fragrance components, humectants, pacifying agents, pH adjusters, plasticizers, preservatives, propellants, reducing agents, skin bleaching agents, skin-conditioning agents (emollients, humectants, miscellaneous, and occlusive), skin protectants, solvents, SPF enhancers/boosters, foam boosters, hydrotropes, solubilizing agents, suspending agents (nonsurfactant), sunscreen agents, ultraviolet light absorbers, water-proofing agents, and viscosity increasing agents (aqueous and nonaqueous).
An emollient is a substance which helps to smooth and soften the skin, and may also reduce its roughness, cracking or irritation. Non-limiting examples of suitable emollients include, for example and without limitation, mineral oil, lanolin oil, coconut oil, cocoa butter, olive oil, almond oil, macadamia nut oil, synthetic jojoba oils, natural Sonora jojoba oils, safflower oil, corn oil, liquid lanolin, cottonseed oil and peanut oil. Preferably, the emollient is a mineral oil NF. One or more emollients may be present ranging in amounts from about 1 percent to about 30 percent by weight.
Other suitable emollients include, for example and without limitation, Aloe Barbadensis Leaf Extract, which is a mixture of Aloe Barbadensis Leaf Extract (&) Cocos Nucifera (Coconut) Oil (&) Mineral Oil. squalane, castor oil, polybutene, sweet almond oil, avocado oil, calophyllum oil, ricin oil, vitamin E acetate, olive oil, silicone oils such as dimethylopolysiloxane and cyclomethicone, linotenic alcohol, oleyl alcohol, the oil of cereal germs such as the oil of wheat germ, isopropyl palmitate, octyl palmitate, isopropyl myristate, hexadecyl stearate, butyl stearate, decyl oleate, acetyl glycerides, the octanoates and benzoates of (C12-C15) alcohols, the octanoates and decanoates of alcohols and poly-alcohols such as those of glycol and glyceryl, ricinoleates esters such as isopropyl adipate, hexyl laurate and octyl dodecanoate, dicaprylyl maleate, hydrogenated vegetable oil, phenyltrimethicone, and jojoba oil.
Other suitable emollients which are solids or semi-solids at ambient temperatures may be used. Such solid or semi-solid cosmetic emollients include, for example and without limitation, petrolatum, glyceryl dilaurate, hydrogenated lanolin, hydroxylated lanolin, acetylated lanolin, isopropyl lanolate, butyl myristate, cetyl myristate, myristyl myristate, myristyl lactate, cetyl alcohol, isostearyl alcohol and isocetyl lanolate. One or more of these emollients can be optionally included in the formulation.
The whipped formulations can further comprise skin protectant active agents. Suitable examples include, for example and without limitation, (with preferred weight percent ranges), Allantoin (0.5 to 2 percent); Aluminum hydroxide gel (0.15 to 5 percent), Calamine (1 to 25 percent); Cocoa butter (greater than 50 percent); Cod liver oil (5 to 14 percent); Dimethicone (1 to 30 percent); Glycerin (20 to 45 percent); Hard fat (greater than 50 percent); Kaolin (4 to 20 percent); Lanolin (12.5 to 50 percent); Mineral oil (greater than 50% percent); Petrolatum/White petrolatum (in certain embodiments, greater than 30% percent); Topical starch (10 to 98 percent); Zinc acetate (0.1 to 2 percent); Zinc carbonate (0.2 to 2 percent); and Zinc oxide (1 to 25 percent), and zinc oxide in ointment (1 to 40 percent). Additional skin protectant active agents may include Colloidal oatmeal or Sodium bicarbonate.
In certain embodiments, water is employed in amounts effective to form the emulsion. It is generally preferred to use water which has been purified by processes such as deionization or reverse osmosis, to improve the batch-to-batch formulation inconsistencies which can be caused by dissolved solids in the water supply. The amount of water in the emulsion or formulation can range from about 15 percent to 95 weight percent. In other embodiments, water is not required.
A humectant is a moistening agent that promotes retention of water due to its hygroscopic properties. Suitable humectants include, for example and without limitation, sorbitol, glycerin, polymeric glycols such as polyethylene glycol and polypropylene glycol, and mannitol. Preferably, the humectant is glycerin, Sorbitol 70% USP or polyethylene glycol 400, NF. More preferably, the humectant is Sorbitol 70% USP. One or more humectants can optionally be included in the formulation in amounts from about 1 percent to about 20 percent by weight, preferably about 3 percent by weight. Other suitable humectants include, inter alia, fructose, glucose, lactic acid, PCA, potassium lactate and PCA, propylene glycol, sodium lactate and PCA.
An antimicrobial preservative may be part of the disclosed formulation. An antimicrobial preservative is a substance or preparation which destroys, prevents or inhibits the proliferation of, microorganisms in the skincare formulation, and which may also offer protection from oxidation. Preservatives are frequently used to make self-sterilizing, aqueous based products such as emulsions. This is done to prevent the development of microorganisms that may grow in the product during the manufacture and distribution of the product and/or during use by consumers, who may further inadvertently contaminate the products during normal use. Typical preservatives include, for example and without limitation, the lower alkyl esters of para-hydroxyben-zoates (parabens), especially methylparaben, propylparaben, isobutylparaben and mixtures thereof, benzyl alcohol, phenyl ethyl alcohol and benzoic acid. The preferred preservative is benzyl alcohol. One or more antimicrobial preservatives can optionally be included in an amount ranging from about 0.001 to about 10 weight percent, preferably about 0.05 to about 1 percent.
An antioxidant may be part of the disclosed formulation. An antioxidant is a natural or synthetic substance added to the sunscreen to protect from or delay its deterioration due to the action of oxygen in the air (oxidation) and to protect the skin from sun damage. Antioxidants prevent oxidative deterioration which may lead to the generation of rancidity and nonenzymatic browning reaction products. Typical suitable antioxidants include, for example and without limitation, propyl, octyl and dodecyl esters of gallic acid, butylated hydroxyanisole (BHA, usually purchased as a mixture of ortho and meta isomers), butylated hydroxytoluene (BHT), nordihydroguaiaretic acid, Oxynex (Oxynex ST liquid is a mixture of diethylhexyl syringyliden-emalonate and caprylic/capric triglyceride), Vitamin A, Vitamin E and Vitamin C. One or more antioxidants can optionally be included in the formulation in an amount ranging from about 0.001 to about 5 weight percent, preferably about 0.01 to about 0.5 percent.
Chelating agents may be part of the disclosed formulation. Chelating agents are substances used to chelate or bind metallic ions, such as with a heterocyclic ring structure so that the ion is held by chemical bonds from each of the participating rings. Suitable chelating agents include, for example and without limitation, ethylene diaminetetraacetic acid (EDTA), EDTA disodium, calcium disodium edetate, EDTA trisodium, citric acid, EDTA tetrasodium and EDTA dipotassium. One or more chelating agents can optionally be included in the formulation in amounts ranging from about 0.001 to about 0.2 weight, percent preferably about 0.01% weight percent.
The disclosed formulation may include foam stabilizers or foam stabilizing agents. There are many examples of such agents and means to achieve foam stability. Non-limiting examples of suitable foam stabilizers include, for example and without limitation, the Avicels, Capmul S12L, Capmul S18L, Amilite GCK-12, Amadol CMA-2, Ampholak 7 CX-C, Ampholak X CO-30, Polyox WSR N-10, Amaranth S, Foam-Coll 5, Blanose 12M31XP, Genu carrageenan, Avanel S150CG and others. Avicel is an example that can be used in the formulation. For example, Avicel RC-591 is a mixture of cellulose gum and microcrystalline cellulose. Some foam stabilizers also help improve long term high temperature stability.
Fragrances are aromatic substances which can impart an aesthetically pleasing aroma to the skincare or sunscreen formulation and may be part of the disclosed formulation. Typical fragrances include, for example and without limitation, aromatic materials extracted from botanical sources (i.e., rose petals, gardenia blossoms, jasmine flowers, etc.) which can be used alone or in any combination to create essential oils. Alternatively, alcoholic extracts may be prepared for compounding fragrances. However, due to the relatively high costs of obtaining fragrances from natural substances, the modern trend is to use synthetically prepared fragrances, particularly in high-volume products. Both types are considered to be within the scope of the present invention.
A pH modifier may be part of the disclosed formulation. A pH modifier is a compound that will adjust the pH of a formulation to a lower, e.g., more acidic pH value, or to a higher, e.g., more basic pH value. The disclosed formulations may contain such pH modifiers as is necessary.
The disclosed whipped formulation product has been developed, in part, to offer consumers a unique and better way to apply topical products such as sunscreen and skin creams to themselves and others.
One advantage of the disclosed whipped formulation product is during dispensing the density of the formulation contained within the package may drop measurably. The resulting dispensed product represents a whipped product (a foam) of substantial rigidity and body, slow to collapse under ambient and elevated temperature conditions but easy to “break” upon physical manipulation, as for example during rubbing. This allows for a more “controlled” and even dispersal/spreading/distribution of product as compared to the initial “un-whipped” presentation of the formulation.
Another advantage of the disclosed whipped product arises from the ability to contain such a large “dispensed volume” in such a condensed package format, allowing for a far more consumer friendly and portable package size/format for such a large volume of dispensed product.
In certain embodiments, the disclosed whipped formulation product can allow for more control of spread over body.
In certain embodiments, the disclosed whipped formulation product allows for high levels of product evacuation, particularly for viscous products as compared to traditional non-pressurized emulsion packaging. In certain embodiments, the disclosed whipped formulation product with its pressured system allows for elevated levels of gas to be dispersed into formulation, beyond what ambient condition would normally allow, which can increase whipping potential (lower resulting dispensed densities) and reduce sputtering that can be caused by dispersing high levels of gas into formulation but failing to provide adequate pressure to contain the dispersed gas. In certain embodiments, the disclosed whipped formulation product results in reduced corrosion potential by separating the formulation from the rigid, pressurized container (if metal) by containing the formulation in the internal bag.
In certain embodiments, the disclosed whipped formulation product can have its gas propellant or combination, pressure, and gas dispersion customized for each formulation. Whereas oil and water emulsions are particularly well suited for specific gases, liquid propellants can provide much larger bubble structures. BOV dispensing mechanism allows for co-blending of the various types of liquid and gas-phase propellant allowing to dispense whipped products without substantially altering temperature or potentially induce a cooling effect due to phase change energy absorption.
The disclosed whipped product is a light and spreadable formulation and thus may be particularly well suited for sensitive or compromised skin applications, such as applying a whipped diaper rash product.
The disclosed whipped product form is designed to dispense, for example and without limitation, lotion/cream/ointment/oral dosage forms/whipped cream in a controlled manner by delivering a pressurized, foaming formulation via a dispensing orifice at the touch of a button. The product is dispensed via an actuator that depresses a valve stem into a female aerosol valve. Upon activation, the gas-saturated formulation experiences a drop in pressure as it moves from a pressurized containment system to ambient conditions. This change in pressure allows the saturated gas to rapidly expand, creating bubbles within the formulation, leading to a formulation of reduced density. Formulation customizations allow these bubbles to remain stable for 10 seconds or longer, permitting the user to spread the resulting product onto a surface with enhanced coverage benefits.
Although specific suppliers of commercially available ingredients may be listed herein, it is understood that these products may be available from additional suppliers and that the instant invention is not limited to only that ingredient from the specifically cited supplier. Rather the supplier is being provided as an example of what is commercially available.
Description of Certain Embodiments of the Whipped Product
In certain embodiments, the formulation is expelled from the package without shaking the package.
Sensory Impact
The disclosed whipped formulation product represents the careful culmination of advancements in formulation, processing, and packaging to deliver a rich, creamy, spreadable, lightweight whipped product for consumer application. The disclosed formulation also delivers desired sensory impact to a user.
Sensory impact (such as appearance of the whipped product, sound upon dispensing the product from the can, and impact on the skin of the whipped formulation, etc.) to the user may be evaluated by, for example, trained personnel to determine how product variants are perceived differently by the user, with statistical confidence. Those formulations determined to have desired sensory impact are thus selected. In certain embodiments, the user's senses are highly satisfied by the disclosed formulation after its application on the user.
Two intertwined process variables may contribute to controlling the consumer experience associated with a base formula; gas loading (e.g., nitrous oxide) into the formulation with the active ingredient, which impacts density, spreadability, sound, and physical appearance of product; and pre-gas can pressure, which influences stability of gas emulsion, sound, speed of dispense, sputtering, and “quality” characteristics. Multiple product variants, combining these two process variables, are run and are being physically evaluated. Physical measurements may be made, including CT scans to yield “in can” product profile characterization details; dispensing observations (such as appearance of the whipped product, sound upon dispensing the product from the can, and impact on the skin of the whipped formulation, etc.), and high temperature foam stability; and post-dispensing physical measurements including density, bubble size, and bubble size distribution. Sensory impact (such as appearance, sound, and skin impact) to the user of these multiple product variants may be evaluated by, for example, trained personnel to determine how product variants are perceived differently by the user, with statistical confidence. Some of these tested whipped formulations would have desired sensory impact to the user. For any given product, the following parameters, as well as any other parameters that impact a user's sense(s), may be evaluated.
Appearance: visual compactness, integrity of shape, gloss, hue, intensity, brightness, opacity, whitening, etc.
Sound impact upon dispensing from the can: volume, tone, crackling/popping, sputtering, etc.
Skin Feel: firmness, stickiness, cohesiveness, peaking, wetness, spreadability, coolness, thickness, slipperiness, oiliness, waxiness, greasiness, rubs to absorbency, tautness, roughness, thickness of residue, grittiness, graininess, chalkiness, peeling/flaking, pilling, powdery-ness, plastic/coated, etc.
In certain embodiments, the whipped formulations have desired sensory impact to a user, who may be a human user. In certain embodiments, the formulations have high sensory impact to the user; in certain embodiments, the high sensory impact is characterized by one or more of the following: positive appearance, low sound impact, high integrity of shape, visual compactness, high spreadability, positive skin feel, afterfeel (immediately after application or after a few minutes after application, such as about 10 minutes after) as well as other sensory input perceivable by a user.
The disclosed method allows for tweaking the consumer experience attributes of a whipped formulation in multiple directions, allowing is to deliver “soft and gentle” or “aggressive and greasy,” etc., depending on consumer preference. Some of the attributes are: appearance, sound impact, integrity of shape, spreadability, and skin feel. All these, as well as other parameters, may be chosen such that the whipped formulation has the desired attributes.
For appearance, in certain embodiments, the appearance is a well-formed dollop; in other embodiments, such as for Kid's Messy-Loud sunscreen, the product upon dispensing sputters.
For sound impact, in certain embodiments, such as Kid's Messy-Loud sunscreen, the sound impact upon dispensing is obnoxiously loud and disruptive; in other embodiments, the sound impact is as low as possible.
For skin feel, in certain embodiments, such as Baby and Clearly Sheer, the skin feel provided by the formulation is a soft, none greasy-feel experience; in other embodiments, such as sunscreen for sport users who want to feel their sunscreen is working hard and staying with them as they move, the skin feel provided is one or more of greasiness, heaviness, and glossy.
In certain embodiments, the disclosed whipped product dispenses in a light whipped form, infused with tiny bubbles that make the texture of the formulation lighter, smoother and easier to spread across the skin. This texture also makes the formulation feel less greasy and more aesthetically pleasing on hands and skin, leaving a ‘sumptuous’ feel with a sunscreen during application. This formulation spreads quickly and disappears rapidly as the user rubs the formulation into the skin. Such a formulation may even prevent excess application of the agent and may offer ecological advantages.
In another embodiment, the disclosed whipped product offers an easier, faster, smoother, and less greasy skincare formulation than a traditional formulation.
In certain embodiments, the physical stability of the whipped products obtained may also be characterized by means of these tests: determination of the organoleptic characteristics (e.g., aspect, color, odor), characterization of the texture (e.g., thick, fluid, greasy, non-greasy), and characterization of the spreadability.
In certain embodiments, the disclosed formulation has one or more of the following physical characteristics: a majority of bubbles being of a bubble size of less than 20 μm, high number of bubbles, high bubble density, and high foam stability. In certain embodiments, the disclosed formulations have high foam stability at high temperatures, such as at 25° C. to 37° C., or 37° C. to 50° C.
In certain embodiments, the color of the whipped formulation post-dispensing is white. The whiteness of the whipped lotion may be used as a visual queue for application on skin.
In certain embodiments, the formulation has at least about 60% of the gas bubbles at ≤100 μm, after the formulation is expelled from the package. In certain embodiments, the formulation has at least about 40% of the gas bubbles at ≤60 μm, after the formulation is expelled from the package.
In certain embodiments, the whipped formulation product is characterized by microdispersion. In certain embodiments, the whipped formulation product is characterized by substantially consistent microvoid.
In certain embodiments, the whipped formulation product is highly emollient. In certain embodiments, the whipped formulation product has about 60% or more of the gas bubbles at ≤100 μm. In certain other embodiments, the whipped formulation product has about 40% or more of the gas bubbles at ≤60 μm. The gas bubbles are formed from the gas propellant co-mingled with the formulation prior to filling the formulation into the package.
In certain embodiments, the formulation has one or more of characteristics such as little or no wetness after application, having a collapse time of at least 60 seconds, or structurally stable for at least 30 minutes. Examples
For this invention to be better understood, the following examples are set forth. These examples are for purposes of illustration only and are not to be construed as limiting the scope of the invention in any manner.
Currently, A+D® Diaper rash products are available as an original ointment and zinc oxide cream. For this study, A+D® zinc oxide cream, which contains 10% w/w zinc oxide, is utilized to explore the feasibility of developing a new whipped delivery system. In addition, the feasibility of developing a whipped 40% (w/w) zinc oxide ointment is evaluated. The whipped zinc oxide cream and ointment evaluated in this study are manufactured and packaged at the intended manufacturing site. Formulation details and brief manufacturing process for the tested whipped products are summarized in Tables 1 through 4.
As summarized in
Accordingly, it is feasible to develop whipped zinc oxide products spanning a large ZnO concentration range, having positive whipped characteristics.
Aloe Barbadensis Leaf
Aloe Barbadensis
Aloe Barbadensis Leaf Extract and
The following progression outlines the major steps involved in the laboratory production of a Whipped embodiment (Finished Product) at ambient temperature.
(1) Gas co-processing step: The concentrate (base formulation) is added to the mixing chamber and a 1st Gas is vigorously co-mingled or dispersed with a high pressure mixing head into the base formulation at 150 psig, and held at pressure until Packaging Step.
(2) Pre-pressurizing step: Pressurizing of a 2nd gas between a bag and the inside wall of the Bag on Valve product package to no less than 40 psig.
(3) Packaging step: Packaging the pre-mixed formulation (concentrate+the 1st gas) into the pre-pressurized Bag on Valve (BOV) package by injection into the two way valve opening at a pressure of at least 400 psig.
In certain embodiments, the following process is used.
1) Concentrate Production Step: The base sunscreen emulsion was processed in accordance with the manufacturing process according to Table 1, and held for the Gas Co-Processing step.
2) Gas Co-Processing Step: The base sunscreen formulation was added to the mixing chamber and a 1st Gas was vigorously co-mingled or dispersed with a high pressure mixing head into the base formulation at 150 psig, and held at pressure until Packaging Step.
3) Pre-pressurizing step: Pressurizing of a 2nd gas between a bag and the inside wall of the Bag on Valve product package to no less than 40 psig.
4) Packaging step: Packaging the pre-mixed formulation (concentrate+the 1st gas) into the pre-pressurized Bag on Valve (BOV) package by injection into the two way valve opening at a pressure of at least 400 psig.
Aloe Barbadensis Leaf
Aloe Barbadensis
The following progression outlines the major steps involved in the laboratory production of a Whipped embodiment (Finished Product) at ambient temperature.
(1) Gas co-processing step: The concentrate (base formulation) is added to the mixing chamber and a 1st Gas is vigorously co-mingled or dispersed with a high pressure mixing head into the base formulation at 150 psig, and held at pressure until Packaging Step.
(2) Pre-pressurizing step: Pressurizing of a 2nd gas between a bag and the inside wall of the Bag on Valve product package to no less than 40 psig.
(3) Packaging step: Packaging the pre-mixed formulation (concentrate+the 1st gas) into the pre-pressurized Bag on Valve (BOV) package by injection into the two way valve opening at a pressure of at least 400 psig.
Two intertwined process variables may contribute to controlling the consumer experience associated with a whipped formulation: (1) gas loading (e.g., Nitrous Oxide), which impacts density, spreadability, sound profile during dispensing, and physical appearance of product; and (2) pre-gas can pressure, which influences stability of gas emulsion, sound, speed of dispense, sputtering, and “quality” characteristics. Multiple product variants, combining these two process variables, were run and were being physically evaluated. Physical measurements were made, including CT scans, to yield “in can” product profile characterization details; dispensing observations (appearance, sound, etc.) and high temperature foam stability; and post-dispensing physical measurements including density, bubble size, and bubble size distribution.
Nine formulations manufactured at various process conditions, representing the practical range of “cut bag” (pre-gas) pressure and nitrous oxide loading, shown in shown in Tables 5 and 7-9 were tested.
Each variable combination sampled was evaluated via a CT Scanner to determine bubble size and bubble size distribution while remaining in-can and under elevated pressure. The samples were then evaluated after dispensing across a wide range of factors including appearance, bubble size and distribution, and high temperature foam stability. The results are shown in
Some post-dispensed results are:
Appearance of “whipped foam”: richer, more voluminous appearance at lower product density (
Gas bubble size and distribution: lower product density leads to higher levels of small bubbles (
High temperature stability: no significant changes in appearance of “whipped foam”, bubble size and distribution at 50° C. (
Changes in cut-bag pressure have minimal effect on “whipped foam” characteristics.
Both the bubble density (
In conclusion, a single finished whipped lotion formulation, processed under a variety of conditions, is capable of possessing unique physical (pre-dispensed and post dispensed) characteristics. Furthermore, these characteristics often translate directly into the consumer experience and have been demonstrated to impact perceptible changes in key consumer criteria including auditory experience, skin feel, perception of the physical characteristics of the product, and application.
Fluid Dynamic Analysis
Fluid dynamic of “in can” product (finished product) was evaluated using CT Scan, which produces cross-sectional images (virtual “slices”) of specific areas of a scanned object, allowing the user to see inside the object without cutting. Density (g/l) means product density (g/L); Cut Bag Pressure (PSIG) means Cut-bag Pressure (psi). Measured precision: Precision of fluid measurement (or CT number precision) was calculated to be: 1 SD: 0.5 HU; Max range: 2 HU. Results are shown in Table 6.
Note: Volall_fluid includes total volume of sample within bag
Whipped sunscreen products consisting of a base emulsion formulation (concentrate) and a propellant (gas) are packaged into a pre-pressurized Bag on Valve (BOV) package. The objective of this example is to evaluate the characteristics of whipped sunscreen products manufactured at various process conditions. Formulation details for a whipped sunscreen product used in the following evaluation studies are summarized in Tables 10 and 11. Batches were prepared based on the whipped sunscreen product SPF 50 at various levels of process conditions: three different cut-bag pressures (20, 32.5, and 45 psi) and three different product densities (50, 125, and 200 g/L). See Table 9. The batches tested in the evaluation studies were manufactured and packaged at the intended manufacturing site.
The results are shown in
Two intertwined process variables may contribute to controlling the consumer experience associated with a base formulation: gas loading (e.g., Nitrous Oxide), which impacts density, spreadability, sound impact upon expelling from the package, and physical appearance of product; and pre-gas can pressure, which influences stability of gas emulsion, sound, speed of dispense, sputtering, and “quality” characteristics. Sensory impact (such as appearance, sound, and skin impact) to the user of product variants of these two variables were evaluated by trained personnel to determine how product variants are perceived differently by the user, with statistical confidence.
The sensory impact studies were conducted by Sensory Spectrum (222 Oak Ave, Kannapolis, NC 28081; 554 Central Ave, New Providence, NJ 07974). These studies involve skinfeel descriptive analysis of a whipped formulation. Whipped formulations with multiple variables are studied to understand impact of modified manufacturing processes on sensory characteristics of the formulation.
Study Design
Protocol Development
Sensory Spectrum consultants and panel leaders evaluate prototypes, method of dispensing/application and sound upon dispensing to develop a custom protocol for descriptive analysis. The Spectrum Descriptive Analysis Method grounds itself in the use of published and internal intensity reference scales to define intensity boundaries in sensory experiences. Skinfeel panelists are trained using the Spectrum Descriptive Analysis Method for personal care products. They are selected on their ability to detect and discriminate differences in visual and tactile properties. Panelists are trained on a universal scale that focuses on intensity or strength of the signal, coupled with detailed description and definitions of sensory attributes and use of calibrated training samples. All panelists receive a minimum of 100 hours of training and practice prior to commissioning of client research and are extensively trained in evaluation of sprays, creams, and related product forms.
Attribute intensity is rated on a 101-point intensity: scale with 0=none and 100=very strong/very high. The intensity scale uses 1-point increments. Panelists are trained to use the scale in a similar way across panelists and across samples. Use of a universal scale allows attributes to be compared in intensity to one another, (e.g. comparing intensity of slippery feel to intensity of sticky feel), as well as for comparison of samples within and across studies and products having shared attributes.
All evaluations are replicated. Data collection of this type is well suited to correlation with both instrumental and consumer research data. The samples are shown in Tables 6, 8, 9, and 10.
The study design involved monadic assessments of whipped sunscreen formulations in a randomized and balanced complete block design, and estimate mean values for each sensory attribute for each product. A trained panel performed all assessments using the Spectrum Descriptive Analysis Method.
The analyses provide both descriptive (qualitative) and intensity measures (quantitative) of the products. The descriptive analysis methodologies are based on those described in ASTM Manual 26, Sensory Testing Methods, 2nd Ed, E. Chambers IV, editor, and ASTM Manual on Descriptive Analysis Testing for Sensory Evaluation, R. Hootman, editor, and Sensory Evaluation Techniques by Meilgard, Civille and Carr.
Prototype Evaluations—Appearance
Sensory Spectrum consultants evaluated the color of the prototypes (hue, intensity, brightness, opacity) via consensus.
Prototype Evaluations—Sound
Sensory Spectrum's Skinfeel Descriptive analysis panel (minimum of eight panelists) was trained to evaluate the volume and pitch of the perceptible sounds of the prototypes as they were dispensed from their containers. They also assessed the presence/absence of qualitative characteristics of the sound.
Prototype Evaluations—Skinfeel Panel Composition: Eight (8) to eleven (11) trained panelists evaluated the products. All panelists passed an annual validation test.
Test Article Description
The sunscreen test articles/products contain sunscreen ingredients that comply with the types, combinations and concentrations specified by the 1999 FDA Final Sunscreen Monograph or subsequent FDA regulations. All products are over-labeled and bulk packaged and/or over-labeled in their marketed packaging. Products that are not sunscreens may also be tested as benchmarks along with the sunscreen test articles/products.
Test Article Description: Whipped Sunscreen SPF 50 Lotion; Sunscreen Lotion SPF 50 Non-Whipped.
Procedures
Two 4″×2″ rectangular evaluation sites were scribed on each volar forearm. Panelists spread the product within the rectangle with index or middle finger, using a gentle oval motion, at a rate of two strokes per second.
Whipped Product Dispensing Instructions:
Pick up can and with other hand twist actuator noting that the icon moves from the locked position to the unlocked. Place index finger into saddle-shaped curve in actuator in preparation to dispense. Rotate can down at an angle, so that the actuator orifice is positioned close (¼ inch) to the petri dish, in preparation to dispense. Depress actuator and allow product to dispense by building into itself on the petri dish and then slowly pull can up and away. Release the actuator after 2 beats of a metronome set at 120 BPM. NOTE: This amount may be enough to cover a whole appendage (arm, leg, or one side of a torso).
Neat Product Dispensing Instructions: In a plastic petri dish, the panel leader or technician dispenses the product from a standard bottle in a spiral shape using a nickel size circle, filling it from the edge to the center.
No adverse events were reported.
The study sampling plan used a randomized and balanced complete block design. Nine samples (Tables 6, 8, 9, and 10) were replicated so that each sample was seen twice by each panelist, and one sample was seen three times by each panelist. The average of the replicate evaluations by each panelist was used in the summary analysis for each attribute. Mean and standard deviation for each attribute was analyzed for each sample. SAS was used to conduct this analysis.
Perceptual maps of the samples were developed to better understand the relationships among the attributes that define the sensory space of the sample category tested and where the products fall in that space. This information is used to group samples in homogeneous groups.
Some of the findings are:
Chroma/Intensity (of Color)
Density appeared to provide a directional impact regarding Chroma and Intensity but statistics were not available.
Cracking/Popping
Both Density and Cut Bag Pressure appeared to provide a directional impact regarding Cracking/Popping noise but statistics were not available.
Sputtering
Both Density and Cut Bag Pressure at lower densities appeared to provide a directional impact regarding Sputtering but statistics were not available.
Noise
Density appeared to provide a directional impact regarding Noise but statistics were not available.
Sound
Overall, many of the samples have a low sound impact when dispensed from the packaging. Three samples are moderately loud and high-pitched. One sample makes a crackling/popping sound while two samples sputter when dispensed.
Three Key Dimensions explain 90% of the variability in descriptive profiles of skinfeel. Dimension 1—Oily during rubout with a glossy thick, greasy residue (53% of variability) Dimension 2—Glossy and low in firmness when dispensed (19% of variability). Dimension 3—Visually compact when dispensed into a petri dish (18% of variability).
Prototypes that stand out in Dimension 1 are as follows. Prototype 836 is oily and slow to absorb during rubout, leaves a moderately glossy finish on the skin, and has the highest, thickest residue that is oily & greasy in character. Prototype 567 absorbs quickly, is less glossy, and leaves a thinner residue.
Prototypes that stand out in Dimension 2 are as follows. When dispensed into a petri dish, Prototype 170 is the shiniest among all prototypes for up to 30 seconds. It is also the least firm when manipulated, but it should be noted that this sample was evaluated slightly differently due to its format (neat, not whipped). Prototype 819 is least glossy when dispensed into a petri dish, and is firmest among the whipped prototypes.
Prototypes that stand out in Dimension 3 are as follows. When dispensed into a petri dish, Prototypes 170 and 903 are visually compact and hold their shape. Prototypes 033, 125 & 567 are airier when dispensed and don't hold their shape as well as other prototypes.
Tables 10-16 display some of the data. Attribute intensity is rated on a 101-point intensity: scale with 0=none and 100=very strong/very high.
6.0 CD
4.8 D
4.8 D
A summary of the study parameters is below.
As it is Dispensed
The foregoing description discloses only exemplary embodiments of the invention.
It is to be understood that while the invention has been described in conjunction with the detailed description thereof, the foregoing description is intended to illustrate and not limit the scope of the invention, which is defined by the scope of the appended claims. Other aspects, advantages, and modifications are within the scope of the appended claims. Thus, while only certain features of the invention have been illustrated and described, many modifications and changes will occur to those skilled in the art. It is therefore to be understood that the appended claims are intended to cover all such modifications and changes as fall within the true spirit of the invention.
| Number | Name | Date | Kind |
|---|---|---|---|
| 3395215 | Schubert et al. | Jul 1968 | A |
| 3710538 | Lowy | Jan 1973 | A |
| 3970584 | Hart et al. | Jul 1976 | A |
| 4670272 | Chen et al. | Jun 1987 | A |
| 5104987 | King | Apr 1992 | A |
| 5214925 | Hoy et al. | Jun 1993 | A |
| 5560859 | Hartmann et al. | Oct 1996 | A |
| 5858343 | Szymczak | Jan 1999 | A |
| 6322776 | Ortega | Nov 2001 | B1 |
| 7070722 | Gilchrist et al. | Jul 2006 | B1 |
| 20040052826 | Fernandez-Kleinlein et al. | Mar 2004 | A1 |
| 20040197270 | Mundschenk | Oct 2004 | A1 |
| 20040241099 | Popp et al. | Dec 2004 | A1 |
| 20040247534 | Stoltz | Dec 2004 | A1 |
| 20040258627 | Riedel et al. | Dec 2004 | A1 |
| 20040258628 | Riedel et al. | Dec 2004 | A1 |
| 20050079142 | Brunckhorst et al. | Apr 2005 | A1 |
| 20080017671 | Shieh et al. | Jan 2008 | A1 |
| 20080138296 | Tamarkin et al. | Jun 2008 | A1 |
| 20080253973 | Tamarkin et al. | Oct 2008 | A1 |
| 20080260655 | Tamarkin et al. | Oct 2008 | A1 |
| 20110281827 | Tamarkin et al. | Nov 2011 | A1 |
| 20120087872 | Tamarkin et al. | Apr 2012 | A1 |
| 20120213712 | Kasai et al. | Aug 2012 | A1 |
| 20120288462 | Lebok et al. | Nov 2012 | A1 |
| 20120288465 | Lechel | Nov 2012 | A1 |
| 20120301422 | Meyer | Nov 2012 | A1 |
| 20130011341 | Nguyen et al. | Jan 2013 | A1 |
| 20130233310 | Hilgers et al. | Sep 2013 | A1 |
| 20140030198 | Fares et al. | Jan 2014 | A1 |
| 20140079648 | Cohen | Mar 2014 | A1 |
| 20140120039 | Baldwin et al. | May 2014 | A1 |
| 20140131395 | Chang | May 2014 | A1 |
| 20160101051 | Tamarkin et al. | Apr 2016 | A1 |
| 20160202051 | Heist et al. | Jul 2016 | A1 |
| 20190142709 | Baldwin et al. | May 2019 | A1 |
| 20190151207 | Baldwin et al. | May 2019 | A1 |
| 20190282464 | Baldwin et al. | Sep 2019 | A1 |
| 20190367256 | Baldwin et al. | Dec 2019 | A1 |
| Number | Date | Country |
|---|---|---|
| 2017263531 | Oct 2018 | AU |
| 2017263533 | Oct 2018 | AU |
| 1217650 | May 1990 | CN |
| 1713891 | Dec 2005 | CN |
| 103547247 | Jan 2014 | CN |
| 110035737 | Jul 2019 | CN |
| 10229812 | Jan 2004 | DE |
| 10304721 | Aug 2004 | DE |
| 1391192 | Feb 2004 | EP |
| 1508326 | Feb 2005 | EP |
| 2319586 | May 2011 | EP |
| 2636401 | Sep 2013 | EP |
| 3454662 | Mar 2019 | EP |
| 3454826 | Mar 2019 | EP |
| 3454946 | Mar 2019 | EP |
| 2560540 | Feb 2016 | ES |
| H3131680 | Mar 1991 | JP |
| H0625051 | Feb 1994 | JP |
| 0103663 | Jan 2001 | WO |
| 2004022019 | Mar 2004 | WO |
| 2005007516 | Jan 2005 | WO |
| 2012154918 | Nov 2012 | WO |
| 2017112727 | Jun 2017 | WO |
| 2017197193 | Nov 2017 | WO |
| 2017197194 | Nov 2017 | WO |
| 2017197195 | Nov 2017 | WO |
| 2017197196 | Nov 2017 | WO |
| 2017197202 | Nov 2017 | WO |
| Entry |
|---|
| International Search Report and Written Opinion received in PCT/US2017/032281 dated Aug. 1, 2017, pp. 16. |
| International Preliminary Report received in PCT/US2017/032281 dated Nov. 13, 2018, pp. 11. |
| Office Action received in U.S. Appl. No. 16/300,323, Jun. 12, 2020, 17 pages. |
| USPTO, Non-Final Rejection of the US Exam Report on U.S. Appl. No. 16/300,342 (Feb. 23, 2023), 15 pages. |
| USPTO, Non-Final Rejection of the US Exam Report on U.S. Appl. No. 16/300,323 (Feb. 8, 2023), 19 pages. |
| Zhang et al., “Nonionic Surfactant Application Patent Technology,” China Light Industry Press, Mar. 31, 2001, pp. 1-2. |
| Chinese National Intellectual Property Administration, Chinese Second Office Action for App. No. 201780028415.1 (Sep. 5, 2022), pp. 1-17. |
| USPTO, Non-Final Rejection of the US Exam Report on U.S. Appl. No. 16/300,342 (Aug. 10, 2022). |
| Chinese Office Action received in 201880031248.0, dated Apr. 18, 2022, pp. 6. |
| Chinese Office Action received in 201780024815.1, dated Dec. 6, 2021, pp. 14. |
| Chinese Office Action received in 201780028486.1, dated Nov. 8, 2021, pp. 12. |
| Food Crumbles, The Science of Foams in Food, Apr. 5, 2020, https://foodcrumbles.com/science-of-foams-in-food (Year 2020), 14 pgs. |
| BPO, Brazilian Office Action received in Brazilian Application No. BR112018073118-8 mailed Nov. 8, 2021, 4 pages. |
| Mexican Patent Office, Mexican Official Action for Mexican App. No. MX/a/2018/013754 (Jun. 22, 2021), pp. 1-6. |
| USPTO, Non-Final Rejection of the US Exam Report for U.S. Appl. No. 16/300,342 (Jun. 24, 2021), pp. 1-13. |
| Dailymed, “Coppertone Defend and Care Oil Free Lotion SPF 30,” www.dailymed.nim.nih.gov. Published online Dec. 17, 2015, pp. 1-3. |
| Australia IP, Examination Report No. 1 for Standard Patent Application for Australian App. No. 2017263538 (Feb. 25, 2021). |
| USPTO, Non-Final Rejection of the US Exam Report for U.S. Appl. No. 16/300,345 (Feb. 5, 2021). |
| USPTO, Non-Final Rejection of the US Exam Report for U.S. Appl. No. 16/300,323 (Jun. 12, 2020). |
| CIPO, Examination Report and Examination Search Report for Canadian App. No. 3,023,714 (Mar. 1, 2021). |
| EPO, Communication Pursuant to Article 94(3) EPC for European App. No. 17726753.1. |
| Australia IP, Examination Report No. 1 for Standard Patent Application for Australian App. No. 2017263531 (Feb. 25, 2021). |
| USPTO, Non-Final Rejection of the US Exam Report for U.S. Appl. No. 16/300,245 (Jul. 23, 2020). |
| USPTO, Final Rejection of the US Exam Report for U.S. Appl. No. 16/300,323 (Nov. 18, 2020). |
| CIPO, Examination Report and Examination Search Report for Canadian App. No. 3,023,669 (Jan. 29, 2021). |
| Australia IP, Examination Report No. 1 for Standard Patent Application for Australian App. No. 2017263532 (Feb. 25, 2021). |
| CIPO, Examination Report and Examination Search Report for Canadian App. No. 3,023,680 (Feb. 17, 2021). |
| EPO, Communication Pursuant to Article 94(3) EPC for European App. No. 17725450.5 (Mar. 19, 2021). |
| Australia IP, Examination Report No. 1 for Standard Patent Application for Australian App. No. 2017263533 (Feb. 25, 2021). |
| CIPO, Examination Report and Examination Search Report for Canadian App. No. 3,023,702 (Feb. 1, 2021). |
| EPO, Communication Pursuant to Article 94(3) EPC for European App. No. 17726754.9 (Feb. 23, 2021). |
| Australia IP, Examination Report No. 1 for Standard Patent Application for Australian App. No. 2017263534 (Feb. 25, 2021). |
| USPTO, Non-Final Rejection of the US Exam Report for U.S. Appl. No. 16/300,342 (Jul. 8, 2020). |
| CIPO, Examination Report and Examination Search Report for Canadian App. No. 3,023,703 (Feb. 12, 2021). |
| EPO, Communication Pursuant to Article 94(3) EPC for European App. No. 17726162.5 (Apr. 2, 2021). |
| EPO, Communication Pursuant to Article 94(3) EPC for European App. No. 17725453.9 (Mar. 19, 2021). |
| USPTO, Non-Final Rejection of the US Exam Report for U.S. Appl. No. 16/300,342 (Dec. 11, 2020). |
| USPTO, Non-Final Rejection of the US Exam Report for U.S. Appl. No. 16/300,289 (Feb. 5, 2021). |
| USPTO, Non-Final Rejection of the US Exam Report for U.S. Appl. No. 16/300,289 (Jul. 27, 2020). |
| International Search Report and Written Opinion received in PCT/US2017/032292 dated Jul. 26, 2017, pp. 10. |
| International Preliminary Report received in PCT/US2017/032292 dated Nov. 13, 2018, pp. 7. |
| Aurena Laboratories, “SunScreen Bag on Valve”, Retrieved from the Internet, Nov. 19, 2014 pp. 1. |
| International Search Report and Written Opinion received in PCT/US2017/032277 dated Aug. 1, 2017, pp. 15. |
| International Preliminary Report received in PCT/US2017/032277 dated Nov. 13, 2018, pp. 10. |
| International Search Report and Written Opinion received in PCT/US2017/032278 dated Jul. 26, 2017, pp. 9. |
| International Preliminary Report received in PCT/US2017/032278 dated Nov. 13, 2018, pp. 6. |
| Mintel, “Hair Styling Foam”, Oct. 2013, XP002772098, Online. |
| Mintel, “Pack Facial Mask”, Mar. 2016, XP002772099, Online. |
| Mintel, “Body Whip Moisture Cream”, Jul. 2008, XP002772100, Online. |
| Mintel, “Body Whip Cream”, Jul. 2008, XP002772101, Online. |
| International Search Report and Written Opinion received in PCT/US2017/032279 dated Jul. 28, 2017, pp. 11. |
| International Preliminary Report received in PCT/US2017/032279 dated Nov. 13, 2018, pp. 8. |
| Number | Date | Country | |
|---|---|---|---|
| 20230233421 A1 | Jul 2023 | US |
| Number | Date | Country | |
|---|---|---|---|
| 62396415 | Sep 2016 | US | |
| 62396424 | Sep 2016 | US | |
| 62351385 | Jun 2016 | US | |
| 62334862 | May 2016 | US |
| Number | Date | Country | |
|---|---|---|---|
| Parent | 16300289 | US | |
| Child | 18126138 | US |
