Pouched product for oral use containing water insoluble base particles - Patents.com

Abstract

A pouched product for oral use comprising a liquid-permeable pouch and a nicotine-containing fill material enclosed in the pouch, the fill material comprising: - the filling material does not contain tobacco or contains tobacco material in an amount of up to 10% of the total weight of the filling material; - having a pre-use moisture content of 1% to 35% of the total weight of the fill material; - containing nicotine in an amount between 0.5% and 2% of the total weight of the fill material; - comprising water-insoluble substrate particles and one or more types of water-soluble components; A pouched product is provided in which the water insoluble base particles are ball-shaped particles constituting at least 65% by dry weight of the fill material, the water insoluble base particles having a d50 particle size of 0.25 mm to 2.0 mm.

Description

[Technical field]

[0001] The present disclosure relates to a pouched product for oral use that includes a liquid permeable pouch and a nicotine containing filling material enclosed in the pouch. [Background technology]

[0002] Oral pouched products as disclosed herein are intended for use in the oral cavity by buccal placement, such as by placing the pouched product between the upper or lower gums and the lips or cheek. Pouched smokeless tobacco products may also be referred to as portion-packed smokeless tobacco products for oral use. Pouched products are typically sized and configured to fit comfortably and discreetly in the user's mouth between the upper or lower gums and the lips or cheek.

[0003] Traditionally, oral pouch-packed products are used in the oral cavity of consumers to deliver active substances such as nicotine, caffeine, and / or different flavors that are beneficial to the user. A common type of nicotine-containing oral pouch-packed product is oral smokeless tobacco products. Such products generally contain additional ingredients such as water, salt, pH adjusters, and flavors and humectants. These products are generally called snuff.

[0004] Buccal pouched nicotine-containing products that are free of tobacco or contain only a small amount of tobacco are currently becoming more and more popular among consumers due to, among other things, their attractive appearance, freshness, and flavor.Furthermore, this type of product allows users to enjoy nicotine without being exposed to tobacco.Buccal pouched products that are free of tobacco or contain little tobacco are usually flavor compositions that contain a filler material, which may include, for example, microcrystalline cellulose or a fiber material derived from a plant other than tobacco.

[0005] Tobacco-free oral pouching products are generally relatively dry products having a pre-use moisture content of less than 35% by weight of the fill material, and often less than 20% by weight of the fill material, although even lower moisture contents, such as between 4 and 15% by weight of the fill material, are known in the art.

[0006] Oral pouching products are typically used by a consumer by placing the pouch between the upper or lower gums and the lips and holding it there for a limited period of time, such as 30 to 45 minutes. The product is configured to fit comfortably and unobtrusively in the user's mouth. The pouch material holds the fill material in place allowing saliva to pass through the pouch material to reach the fill material and allowing flavors and actives, such as nicotine, to leach from the fill material and diffuse from the fill material into the consumer's mouth. [Prior art documents] [Patent documents]

[0007] [Patent Document 1] International Publication No. 2012 / 069505 [Non-patent literature]

[0008] [Non-Patent Document 1] Federal Register / vol.74, no. 4 / 712-719 / Wednesday, January 7, 2009 / Notices “Total moisture determination” [Non-Patent Document 2] AOAC (Association of Official Analytical Chemics), Official Methods of Analysis 966.02: "Moisture in Tobacco" (1990), Fifth Edition, K. Helrich (ed) Summary of the Invention [Problem to be solved by the invention]

[0009] It is an object of the present disclosure to provide an oral pouched nicotine product containing a fill material having improved nicotine release characteristics.A further object is to provide an oral pouched nicotine product that provides improved user satisfaction.A further object is to provide an oral pouched nicotine product that provides improved mouthfeel. [Means for solving the problem]

[0010] One or more of the above objects may be achieved by a buccal pouched nicotine product as claimed in claim 1. Modifications of the present disclosure are set out in the dependent claims and in the following description.

[0011] A pouched product for oral use as disclosed herein comprises a liquid permeable pouch and a nicotine-containing fill material enclosed in the pouch, the fill material being - be a filling material that does not contain tobacco or that contains tobacco material in an amount up to 10% by weight of the total weight of the filling material; - having a pre-use moisture content of 1% to 35% of the total weight of the fill material; - containing nicotine in an amount between 0.5% and 2% of the total weight of the fill material; - comprising water-insoluble substrate particles and one or more types of water-soluble components; The water insoluble base particles are ball-shaped particles which constitute at least 65% by dry weight of the filler material, the water insoluble base particles having a d50 particle size of 0.25 mm to 2.0 mm.

[0012] The water insoluble substrate particles may have a d50 particle size between 0.3 mm and 2.0 mm, such as 0.3 mm to 1.5 mm, 0.3 mm to 1.0 mm, or 0.25 mm to 1.0 mm.

[0013] The water insoluble substrate particles may have a d50 particle size between 0.25mm and 0.6mm, or 0.3mm and 0.6mm, preferably 0.3mm and 0.5mm.

[0014] Additionally, the water insoluble substrate particles may have a d50 aspect ratio of 0.8 or greater and a d50 sphericity of 0.8 or greater.

[0015] The d50 particle size can be determined, for example, using a QicPic image analyzer ID No. 290-D, from Sympatec GmbH, 2012, equipped with a Rodos / L dispersion line ID NO 214D and a Vibri / L sample supply ID NO 273, or an equivalent instrument.

[0016] The d50 aspect ratio and d50 sphericity can be determined, for example, using a QicPic image analyzer ID No. 290-D from Sympatec GmbH, 2012, equipped with a Rodos / L dispersion line ID NO 214D and a Vibri / L sample supply ID NO 273, or an equivalent instrument.

[0017] The pouched products for oral use disclosed herein may have a nicotine release profile such that after a 10 minute usage period, 30% or more, preferably 40% or more of the nicotine in the product has been released, and after a 30 minute usage period, 40% or more, preferably 50% or more of the nicotine in the product has been released.

[0018] The water insoluble substrate particles may comprise or consist of particles of microcrystalline cellulose (MCC), water insoluble starch, silica or mixtures thereof.

[0019] It may be preferred that the water-insoluble substrate particles comprise or consist of particles of microcrystalline cellulose.

[0020] The water insoluble substrate particles may constitute 65% to 99% by dry weight of the filler material, preferably 75% to 95% by dry weight of the filler material, and more preferably 85% to 95% by dry weight of the filler material.

[0021] The fill material in an oral pouched product having a relatively low pre-use moisture content as disclosed herein may be perceived by the user as fresh and pleasant to handle when removed from the user container and placed in the mouth.

[0022] It may be preferred that the moisture content of the fill material in the oral pouched products disclosed herein be 20% by weight or less, or even 15% by weight or less.

[0023] It may be preferred that the water insoluble substrate particles, and preferably also the filler material that comprises the water insoluble substrate particles, contain a low amount of fines.

[0024] The water insoluble substrate particles may include less than 0.5% by weight of particles that pass through a sieve having a mesh size of 250 μm.

[0025] It may further be preferred that the filler material contains less than 0.5% by weight of particles passing through a sieve having a mesh size of 250 μm.

[0026] A mesh size of 250 μm corresponds to a particle size of small to medium sized sand particles, which can be very unpleasant if they leak through the cover material into the mouth of the user after the product is placed in the mouth, causing a rough, dry mouth feel that can persist for an extended period of time, especially if the particles are non-dissolving particles.

[0027] The water-insoluble substrate particles are preferably of substantially the same size and have a narrow particle size distribution. A particulate material consisting of ball-shaped particles having a generally spherical shape and a narrow particle size distribution has a predictable packing pattern and bulk volume, and the void volume in the particulate material remains substantially constant even if the particles shift position within the liquid-permeable pouch as, for example, the result of mechanical action of the pouch by the user when the pouch is forced into place in the mouth.

[0028] Filling materials as disclosed herein may include a sugar alcohol such as maltitol, mannitol or isomalt, or a combination of two or more different sugar alcohols.

[0029] The filling material as disclosed herein preferably comprises up to 15% sugar alcohol by dry weight of the filling material, preferably up to 10% sugar alcohol by dry weight of the filling material, and most preferably less than 5% sugar alcohol by dry weight of the filling material. The filling material may be free of sugar alcohol.

[0030] It may be particularly preferred that substantially all of the nicotine in the fill material is disposed on the outer surface of the water-insoluble substrate particles. In the oral pouched products disclosed herein, it may be preferred that at least 85% of the nicotine, such as at least 90% of the nicotine, is disposed on the outer surface of the water-insoluble substrate particles.

[0031] By concentrating the nicotine on the surface of the water-insoluble substrate particles, the nicotine is distributed non-uniformly throughout the fill material and is readily available for dissolution into the saliva that flows into the interstices between the water-insoluble substrate particles. This is in contrast to substrate particles where the nicotine is absorbed into the structure of the substrate particle or mixed into the substrate material that is formed into particles by a process such as extrusion.

[0032] The one or more types of water-soluble components and other additives are preferably applied to the water-insoluble base particles of the water-insoluble particulate material in the filler material after the water-insoluble base particles are formed. The one or more types of water-soluble components and other additives can be added to the water-insoluble base particles as a liquid / aqueous mixture. All added components can be included in the same mixture. Alternatively, different components can be added in different application steps, for example, a flavolant can be added in a separate step from an active agent such as nicotine. By adding the one or more water-soluble components and other additives to the pre-formed water-insoluble base particles, most of the additives remain on or in the surface of the water-insoluble base particles and do not penetrate into the interior of the water-insoluble base particles, so that all or substantially all of the additives are present on or in the surface of the water-insoluble base particles in the filler material. The water-insoluble base particles are preferably homogeneous hydrophilic particles, such as particles of one or more of microcrystalline cellulose, water-insoluble starch, and silica. It may be more preferred that the water-insoluble base particles are composed of one or more monocomponent particles of microcrystalline cellulose, water-insoluble starch, and silica. Microcrystalline cellulose may be particularly preferred due to the ready availability of food grade varieties.

[0033] The pouched product as disclosed herein may have a liquid-permeable pouch with a filling degree of 80% or less, preferably 75% or less, as measured according to the method disclosed herein. By leaving room for the water-insoluble substrate particles to move within the liquid-permeable pouch, nicotine release may be promoted by moving the water-insoluble substrate particles within the pouch, thereby exposing new particles to saliva. Furthermore, oral pouched products with a relatively low filling degree, such as 80% or less, are more malleable than tightly packed pouches and have a higher conformability to the space between the lips and gums of the user. The generally spherical, ball-like water-insoluble substrate particles contribute to the malleability of the oral pouched product, since the particles can shift position within the pouch with little friction due to the minimal contact area between the particles. The oral pouched product may therefore be perceived by the user as easier to push into place under the lips and more comfortable to use than oral pouched products with less malleability.

[0034] The liquid permeable pouch may be formed from a nonwoven material, such as a nonwoven material comprising regenerated cellulose staple fibers. Nonwoven materials, such as bonded carded webs of regenerated cellulose staple fibers, are well suited for use in liquid permeable pouches as disclosed herein because they are hydrophilic, allowing saliva to move in and out of the pouch and even be absorbed and transported along the fibers in the material.

[0035] Nicotine may be added to the water-insoluble substrate particles of the filler material in the form of a nicotine compound. The nicotine compound may be nicotine base and / or may be selected from nicotine hydrochloride, nicotine dihydrochloride, nicotine monotartrate, nicotine bitartrate, nicotine bitartrate dihydrate, nicotine sulfate, nicotine zinc chloride monohydrate, and nicotine salicylate, nicotine benzoate, nicotine polacrilex, and any combination thereof.

[0036] The filling material of the oral pouching product disclosed herein is a tobacco-free filling material or a filling material with a low tobacco content, the filling material containing tobacco material in an amount of at most 10%, preferably 0.05% to 1%, based on the total weight of the filling material. In such a case, the tobacco material may be a nicotine source. The water-insoluble substrate particles in the filling material as disclosed herein are preferably constituted by tobacco-free particles such as microcrystalline cellulose, water-insoluble starch, silica, or a mixture of two or more different types of tobacco-free particles. Filling materials or water-insoluble substrate particles containing only a trace amount of tobacco, less than 0.05% of the total weight of the filling material, are considered to be tobacco-free.

[0037] The fill material described herein may further comprise an additive selected from the group consisting of pH adjusters, flavors, sweeteners, humectants, and any mixture thereof. The additive may be a flavor, such as synthetic flavors, botanical flavors, flavor oils, hydrophobic flavor oils such as essential oils, for example, nature-identical flavors. As used herein, nature-identical flavors are synthetic flavors that are chemically identical to natural flavors, but are prepared or extracted using chemical methods. The flavor may be a mixture of different flavors. The flavor may be stable at pH>7. Furthermore, the flavor of the fill material in the oral pouched nicotine product described herein may be a hydrophobic flavor, such as hydrophobic flavor oils.

[0038] Examples of flavors include bergamot, eucalyptus, orange, mandarin, citrus, lemon, peppermint, spearmint, mint, menthol, licorice, wintergreen, whiskey, rum, cherry, various berries, tobacco, coffee, vanilla, lime, apple, peach, carvone, limonene, and any combination of two or more thereof. In one example, the flavor comprises a tobacco flavor.

[0039] The fill material of the buccal pouched nicotine products described herein may contain flavoring in the range of about 0.5% to about 3.0% by weight based on the total weight of the fill material.

[0040] The humectant may be glycerol and / or propylene glycol. The sweetener may be an artificial sweetener.

[0041] With respect to particle size, one preferred embodiment of the pouched product for oral use disclosed herein comprises a liquid-permeable pouch and a nicotine-containing fill material enclosed in the pouch, the fill material being - the filling material does not contain tobacco or contains tobacco material in an amount of up to 10% of the total weight of the filling material; - having a pre-use moisture content of 1% to 35% of the total weight of the fill material; - containing nicotine in an amount between 0.5% and 2% of the total weight of the fill material; - comprising water-insoluble substrate particles and one or more types of water-soluble components; the water insoluble base particles are ball-shaped particles constituting at least 65% by dry weight of the filler material, the water insoluble base particles having a d50 particle size of 0.3 mm to 0.6 mm, preferably 0.3 mm to 0.5 mm; The water insoluble substrate particles comprise less than 0.5% by weight of the particles that pass through a sieve having a mesh size of 250 μm.

[0042] With respect to particle size, another preferred embodiment of the pouched product for oral use disclosed herein comprises a liquid-permeable pouch and a nicotine-containing fill material enclosed in the pouch, the fill material being - the filling material does not contain tobacco or contains tobacco material in an amount of up to 10% of the total weight of the filling material; - having a pre-use moisture content of 1% to 35% of the total weight of the fill material; - containing nicotine in an amount between 0.5% and 2% of the total weight of the fill material; - comprising water-insoluble substrate particles and one or more types of water-soluble components; the water insoluble base particles are ball-shaped particles constituting at least 65% by dry weight of the filler material, the water insoluble base particles having a d50 particle size of 0.3 mm to 0.6 mm, preferably 0.3 mm to 0.5 mm; The filler material contains less than 0.5% by weight of particles passing through a sieve having a mesh size of 250 μm.

[0043] definition The terms "oral" and "oral use" refer to the use of a product in contact with the mucous membranes in the human oral cavity, such as buccal placement of the product in the oral cavity. Products for oral use as disclosed herein are intended to be placed in their entirety in the oral cavity and are not intended to be swallowed.

[0044] As used herein, the term "pouched product for oral use" or "oral pouched product" refers to a portion of a smokeless composition containing saliva-extractable matter contained within a saliva-permeable pouch, which is generally made from a flexible, saliva-permeable material, such as a nonwoven material.

[0045] As used herein, a "particle" is a three-dimensional piece of material having a maximum dimension of less than 5 mm and an aspect ratio of 0.3 to 1. R is calculated as the width w of the particle divided by the length l of the particle, where the length is determined as the largest dimension of the particle and the width is determined as the largest dimension perpendicular to the length, i.e., A R = l / w. Particles with an aspect ratio of 1 can be, for example, perfect spheres or cubes. Particles useful as particulate materials in the filling materials of the oral pouching products disclosed herein have a generally spherical shape, referred to herein as "ball-like", with an aspect ratio of 0.8 or greater. The particles can have a generally smooth outer surface or can have microscopic irregularities within the outer surface.

[0046] As used herein, the expression "narrow particle size distribution" intends that the diameter of the particles varies by no more than ±30%, preferably no more than ±20%, and most preferably no more than ±10%. The particle size distribution and shape can be determined by image analysis using a dynamic image analyzer such as the QicPic device from Sympatec GmbH.

[0047] The diameter of the water-insoluble substrate particle as described herein can be calculated as the diameter of the circle of equal projected area, which is the diameter of the circle that has the same area as the projected area of ​​the particle.In this context, projected area is the area resulting from the two-dimensional projection of a three-dimensional particle.As described herein, image analysis can be used to determine the diameter of the particle as described herein.Image analysis can be carried out using the device of Sympatec GmbH as described herein.

[0048] The term "d10", "d50", "d90", or "d10 value", "d50 value", "d90 value" as used herein refers to the value of particle diameter in the cumulative distribution of a group of particles with respect to volume. For example, if d50=0.8 μm, 50% of the particles in the sample have a diameter larger than 0.8 μm, i.e., larger than 0.8 μm, and 50% of the particles in the sample have a diameter smaller than 0.8 μm, i.e., smaller than 0.8 μm. Thus, d50 is the median of the particle size distribution. In a further example, if d10=0.8 μm, 10% of the particles have a diameter smaller than 0.8 μm. If d90=0.8 μm, 90% of the particles have a diameter smaller than 0.8 μm. The two values ​​of d10 and d90 define the range of particle sizes of a particle sample. A small number of particles with diameters outside the range defined by d10 and d90 can be ignored. A sample with a narrow particle size distribution has a d90 / d10 ratio of 1, or about 1.

[0049] The circularity of a particle is the ratio of the average radius of curvature of all convex regions to the circumscribing circle of the particle, and is given by the formula

[0050]

number

[0051] is calculated according to Where: R = radius of circumscribed circle r i = radius of the inscribed circle at convex corner i.

[0052] Sphericity, S, which may be denoted as “S”, is a measure of how close a particle is to a mathematically perfect sphere. Sphericity, S, is the perimeter of an equivalent circle, P EQPC and actual perimeter P real The ratio of the perimeter of the equivalent circle P EQPC is the perimeter of a circle having the same area as the projected area of ​​the particle. In this context, the projected area is the area resulting from the two-dimensional projection of a three-dimensional particle. A particle with a sphericity value S equal to 1 has the shape of a perfect sphere. Sphericity can be calculated based on measurements using image analysis results on a sample of the particle, and is given by the projected area A and the projected actual perimeter P real The image analysis can be carried out using an instrument from Sympatec GmbH as described herein. The sphericity is calculated according to the formula:

[0053]

number

[0054] It can be calculated according to:

[0055] The ball-shaped particles as disclosed herein may be particles having an aspect ratio of 0.8 or more and a sphericity of 0.8 or more in combination. The ball-shaped particles as disclosed herein may further be particles having a circularity of 0.4 or more in combination with an aspect ratio of 0.8 or more and a sphericity of 0.8 or more. As mentioned herein, these parameters may be measured by a dynamic image analyzer from Sympatec GmbH or an equivalent device.

[0056] "Water-insoluble particles" as referred to herein are particles that do not dissolve when exposed to saliva in the mouth of a user, and retain or substantially retain their shape when incorporated into a pouched product for oral use.Water-insoluble also implies that the particle size of the water-insoluble substrate particles as referred to herein does not decrease, or at least does not decrease by more than 1% during use of the oral pouched product incorporating the water-insoluble substrate particles. The shape and particle size of the water-insoluble substrate particles can be substantially unaffected during use. However, a certain amount of swelling of the water-insoluble substrate particles can occur. The swelling should preferably be less than 30% of the pre-use bulk volume of the water-insoluble substrate particles, and more preferably be less than 20% of the pre-use bulk volume of the water-insoluble substrate particles.

[0057] As used herein, the term "moisture content" refers to the weight percent, wt%, of oven volatiles, such as water and other oven volatiles (e.g., propylene glycol), present in a component material, composition, or product, as determined according to the Loss on Drying (LOD) method disclosed herein.

[0058] The "dry weight" of an ingredient, composition, or product is calculated by subtracting the moisture content from the total weight of the ingredient, composition, or product, where the moisture content is determined by the Loss on Drying (LOD) method disclosed herein.

[0059] The term "additional ingredient" refers to any ingredient other than water that is present in addition to the particles of particulate material in the fill material as disclosed herein, such as salts (e.g., sodium chloride, potassium chloride, magnesium chloride, calcium chloride, and any combination thereof), pH adjusters (e.g., sodium hydroxide, potassium hydroxide, potassium carbonate, sodium carbonate, or sodium bicarbonate), flavors, sweeteners, colorants, humectants (e.g., propylene glycol or glycerol), antioxidants, preservatives (e.g., potassium sorbate), binders, tobacco and non-tobacco plant materials, etc. The one or more types of water-soluble ingredients that are part of the fill material in the oral pouching products as disclosed herein constitute the one or more additional ingredients.

[0060] The term "flavor" or "flavoring" is used herein for substances used to affect the aroma and / or taste of oral pouched products. Flavors may be food grade natural or synthetic flavors as known in the art and may include, but are not limited to, essential oils, single flavor compounds, blended flavor substances, and extracts.

[0061] "Tobacco" or "tobacco material" means any part of any species of the genus Nicotiana, including leaves, stems, stalks, and flowers.

[0062] "Cover material" as used herein means any suitable saliva-permeable packaging material as known in the art. Cover material, also referred to as "pouch material", can be a material made by conventional fiber production methods such as nonwoven material, weaving or knitting, or can be an apertured plastic film or netting. Nonwoven materials suitable for use as cover materials may be nonwoven materials comprising staple fibers such as regenerated cellulose staple fibers, e.g., viscose rayon staple fibers or lyocell fibers, and chemical binders such as polyacrylate binders. Such nonwoven materials are generally produced by combing staple fibers to form a fibrous web, and then consolidating the combed fibrous web with a binder. Alternatively, nonwoven materials may include fibers formed into a nonwoven web by spunbonding, hydroentangling, meltblowing, and the like. The fibers used in such processes are generally thermoplastic fibers that are thermally bonded to form a coherent nonwoven web. The coating material may optionally include additional ingredients such as fragrances and / or colorants.

[0063] A common method of making pouched products having a generally rectangular pillow-like shape is to provide the cover material as a seamless endless tube or to form a flat web of cover material into an endless tube with a continuous seal along the length of the tube. The endless tube is then intermittently sealed across the tube while the endless tube is filled with a filler material and placed into pockets formed between the transverse seals. Individual pouched products are cut from the filled and sealed tube of cover material and are typically packaged in user containers. Sealing of the cover material can be accomplished using any suitable method or combination of methods, such as with adhesives, heat sealing, ultrasonic welding, needling, and the like. Heat sealing and ultrasonic welding require that the cover material contain at least a functional amount of a thermoplastic material, such as a thermoplastic fiber or a thermoplastic binder.

[0064] Pouched products for oral use are usually sized and configured to fit comfortably and unobtrusively in the mouth of a user between the upper or lower gums and the lips. The most common shape of pouched products for oral use is a pillow shape, commonly referred to as a "rectangular shape", based on the flat shape of the saliva-permeable pouch before filling. Pouched products for oral use may have a maximum length measured in the longitudinal direction of the product in the range of 25 mm to 40 mm, and a maximum width measured in the transverse direction of the product in the range of 5 mm to 20 mm. The maximum width of an oral pouched product is generally the width of the product as measured along the end seal. The pre-use thickness of a pouched product is usually in the range of 2 mm to 8 mm. The total weight of a pouched product for oral use is typically in the range of about 0.3 g to about 3.5 g, such as about 0.5 g to 1.7 g per pouched product. The volume of the portion of the filling material in the pouch is generally about 0.5 cm, depending on the size of the pouch. 3 From 1.5cm 3 is within the range.

[0065] A "user container" is a consumer package having a shape and size adapted to facilitate carrying the user container in a pocket or handbag. A user container typically contains between 10 and 30 oral pouched products. The pouched products may be randomly placed in the user container or may be arranged in some pattern, for example as disclosed in International Publication No. WO 2012 / 069505 A1. The user container may include a waste compartment for storing used oral pouched products. The waste compartment is separate from a compartment within the container in which fresh, unused, oral pouched products are stored until they are used.

[0066] The amount of nicotine in the fill material may be from 0.6% to 1.7%, or from 0.8 to 1.4%, or from 1.0 to 1.2%, based on the total weight of the fill material.

[0067] The invention is further explained below, by way of non-limiting examples, with reference to the accompanying drawings, in which: [Brief description of the drawings]

[0068] [Figure 1] FIG. 1 shows a pouched product for oral use. [Diagram 2] FIG. 2 illustrates a portion of the fill material within the pouched product of FIG. 1. [Diagram 3] FIG. 1 illustrates a testing device used in determining the fill level of oral pouched products. [Figure 4] FIG. 1 is a schematic diagram showing an image analysis device. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0069] The pouched product for oral use 1 shown in Figure 1 comprises a liquid permeable covering material 2 and a portion-sized amount of fill material 3 comprising a plurality of water-insoluble substrate particles 4 encapsulated in the liquid permeable covering material 2. The cover material 2 may be any suitable type of cover material as disclosed herein and is formed into a generally rectangular pouch into which the fill material 3 is inserted.

[0070] A common method of making pouched products having a generally rectangular pillow-like shape, such as pouched product 1 shown in FIG. 1, is to provide the cover material as a seamless endless tube or to form a flat web of cover material into an endless tube with a continuous seal along the length of the tube. The endless tube is then intermittently sealed across the tube while the endless tube is filled with a fill material into pockets formed between the transverse seals. Individual pouched products are cut from the filled and sealed tube of cover material and are typically packaged in user containers. Sealing of the cover material can be accomplished using any suitable method or combination of methods, such as with adhesives, heat sealing, ultrasonic welding, needling, and the like. Heat sealing and ultrasonic welding require that the cover material include at least a functional amount of a thermoplastic material, such as a thermoplastic fiber or a thermoplastic binder.

[0071] The longitudinal seals formed during manufacture appear as longitudinal seals 6 extending along the length l of the pouched product 1 shown in Figure 1. If the cover material is provided in the form of a seamless, endless tube, no such seals are present. The transverse seals form end seals 7 that define the width w of the pouched product 1. The pouched product 1 has a first major surface 8 and a second major surface 9, with a thickness t defined as the maximum vertical distance between the first major surface 8 and the second major surface 9.

[0072] The particles 4 of the water-insoluble particulate material, as described herein, may constitute a very high percentage of the total dry weight of the filler material 3, such as from 65% to 99% by dry weight of the filler material.

[0073] The fill material 3 further comprises one or more types of water soluble ingredients 11, such as flavors, sweeteners, active ingredients such as nicotine, etc., as disclosed herein.

[0074] A portion of a fill material 3 for an oral pouched product as disclosed herein is shown in FIG. 2, and includes a plurality of generally spherical, ball-like water-insoluble substrate particles 4 having a thin layer of a water-soluble component on the surface of the particles 4.

[0075] As discussed herein, the particles 4 of the filler material have a relatively large d50 particle size in the range of 0.25 mm to 2.0 mm.

[0076] 2 shows only a very small number of particles 4. In a complete portion of the filling material 3 for the oral pouched product 1, the number of particles 4 of the water-insoluble particulate material is much higher, such as on the order of 150 particles or more, which means that the majority of the particle surface is located within the interior of the filling material 3.

[0077] Test Method Methods for determining moisture content, loss on drying, LOD Moisture content as referred to herein can be determined using a method based on the document Federal Register / vol.74, no. 4 / 712-719 / Wednesday, January 7, 2009 / Notices "Total moisture determination" and AOAC (Association of Official Analytical Chemics), Official Methods of Analysis 966.02: "Moisture in Tobacco" (1990), Fifth Edition, K. Helrich (ed). In this method, moisture content is determined gravimetrically by taking a sample of 2.5±0.25 g before water evaporation and after dehydration is complete, and weighing the sample under environmental conditions, defined herein as a temperature of 22° C. and a relative humidity of 60%. Mettler Toledo's Moisture Analyzer HB43, a balance using halogen heating technology, is used in the experiments described herein (instead of an oven and balance as in the aforementioned document). The sample is heated to 105°C (instead of 99.5±0.5°C as in the aforementioned publication). The measurement is stopped when the weight change is less than 1 mg within a 90 second time frame. The weight percent moisture content of the sample is then automatically calculated by the Moisture Analyzer HB43.

[0078] Method for determining particle size and shape by image analysis Particle circularity, particle sphericity, aspect ratio, and particle size were determined using a QicPic image analyzer ID No. 290-D, Sympatec GmbH, 2012, equipped with a Rodos / L dispersion line ID No. 214D and a Vibri / L sample feed ID No. 273, or equivalent equipment. The well-dispersed particle stream is passed through the image plane of the measurement device, as shown in Figure 4, where 21 is a pulsed light source, 22 is a beam expansion unit adaptable to the measurement range, 23 is a dispersion unit, 24 is the particle stream, 25 is a lens, and 26 is a camera. If the particles are small, a large number of particles can be captured per image frame, such as on the order of 50,000 to 100,000 particles per image frame. For larger particles, such as particles having a size of 300 μm to 3000 μm, the number of particles per image frame may be substantially less, on the order of 300 to 2000 particles per image frame.

[0079] Sieve method Commercially available particle sieving equipment such as a Retsch / AS 200 controlled vibrating sieve may be used. A 10 g sample of the tested filler material or water-insoluble substrate particles is placed on a sieve, such as a sieve with a mesh size of 250 μm, and vibrated for 1 minute with an amplitude of 1 mm.

[0080] The weights of the upper and lower fractions of the sample are determined and these weights are used to calculate the percentage of the sample that passed through the mesh.

[0081] Method for determining the degree of fill in oral pouched products Measurements are performed under ambient conditions, as defined herein. Pouch 1 is mounted in frame 20 with first transverse end seal 7' under second transverse end seal 7''. Pouch 1 is attached to frame 20 using double-sided tape attached to first transverse end seal 7'. Frame 20 is designed to support filled pouch 1 without compressing it. After mounting the filled pouch in the frame, the shortest distance between the upper surface of fill material 3 and first transverse seal 7', i.e., the height of fill material 3 within pouch 1, is determined using a digital tabletop caliper device with a resolution of 0.01 mm. A background LED light may be directed at pouch 1 for improved content identification. Care should be taken not to agitate or shake filled pouch 1 when mounting the pouch in the frame.

[0082] The fill level of a mouth pouched product is calculated by dividing the measured height of the fill material in the pouch by the inside distance between the first and second transverse end seals 7', 7'' and is reported as a percent (%) of the available fill height.

[0083] (Example) Sample preparation Five different MCC materials were tested, as shown in Table 1.

[0084] [Table 1]

[0085] The tested materials according to Examples 1 and 2 and References 1 and 2 had sphericity, aspect ratio and particle size as shown in Table 2, measured at d50 using an image analyzer from Sympatec GmbH. The materials according to Examples 1 and 2 contained less than 0.5% by weight of particles passing through a sieve with a mesh size of 250 μm.

[0086] [Table 2]

[0087] For each sample, a solution was prepared from 48.3 grams of 20% nicotine in glycerin (supplied by CNT, Germany), 6.5 grams of potassium carbonate, 15 grams of sodium chloride, 1 gram of acesulfame K, and 110.3 grams of water.

[0088] This nicotine-containing solution was then mixed with 809 grams of the MCC material to be tested and 10 grams of peppermint flavor. The mixture was allowed to stand at room temperature without stirring for 16 hours, resulting in nicotine-containing particles.

[0089] Particles of the five different sample materials were then packed into rectangular pouches with a width w of 12.5 mm and a length l of 37 mm, as shown in Figure 1. The inner length of the pouch between the end seals 7 was 32 mm. Each pouch was filled with nicotine-containing particles to a filling level of approximately 65.6%.

[0090] The pouch material used for all samples was standard viscose nonwoven No. Z8732 from TENOWO GmbH.

[0091] Test procedure Seven subjects were each given five containers, each containing two sample products with one of the test fill materials, for a total of ten sample products per subject. Subjects were also given ten glass vials to store the samples in after use. Each vial was labeled with the sample that was to be placed in the vial, e.g., "Example 1, 10 minutes" or "Reference 3, 30 minutes."

[0092] Subjects were instructed not to use any tobacco products or other nicotine-containing products for at least 30 minutes prior to each test and to rinse their mouths with water before testing. Subjects were instructed to use the sample products in their usual manner, but were instructed not to consume any food or drink during the test period.

[0093] The test was performed by subjects in the following manner. 1. Randomly select a vial and check the label to understand which sample goes in the vial. 2. Remove the sample from the container that holds it according to the label on the vial. 3. Place the sample under your lip and leave it there for 10 or 30 minutes, depending on what is written on the label of the vial that the sample comes in after use. 4. After using the sample product, carefully remove the sample product with tweezers, avoiding squeezing the sample. 5. Place used sample product into assigned glass vial. 6. Store the glass vials in the freezer until all sample product has been used.

[0094] The used samples were then analyzed to determine the nicotine content. Unused samples were also analyzed to determine the original nicotine content. The filling materials of Example 1 and Example 2 were found to have a nicotine release profile such that after 10 minutes more than 30% of the nicotine was extracted, and after 30 minutes more than 40% of the nicotine was extracted. The filling material of Example 2 using water-insoluble ball-shaped MCC particles with a particle size (d50) of 445 μm was found to have surprisingly good nicotine release properties, with about 40% of the nicotine already released after 10 minutes, and more than 55% of the nicotine released after 30 minutes. The filling material using water-insoluble ball-shaped MCC particles with a particle size (d50) of 890 μm was also found to have good nicotine release properties, with a percentage of nicotine released slightly more than 30% after 10 minutes, and more than 45% after 30 minutes.

[0095] All reference samples showed fairly low nicotine release after 10 minutes, with only Reference 2 reaching an acceptable level of nicotine release after 30 minutes.

[0096] These results are shown in Table 3 below.

[0097] [Table 3] [Explanation of symbols]

[0098] 1. Pouched products for oral use 2 Liquid-permeable cover material 3 Filling material 4 Water-insoluble base material particles 6 Longitudinal seal 7 End seal 7' First transverse end seal 7'' Second Transverse End Seal 8 First main surface 9 Second main surface 11 Water-soluble components 20 Frames 21 Pulsed Light Source 22 Beam expansion unit 23 Distributed Units 24 Particle flow 25 Lenses 26 Camera

Claims

1. 1. A pouched product for oral use comprising a liquid permeable pouch and a nicotine-containing fill material enclosed in said pouch, said fill material comprising: - a filling material that is tobacco-free or that contains tobacco material in an amount of up to 10% of the total weight of said filling material; - has a pre-use moisture content of between 1% and 35% of the total weight of said filling material, - containing nicotine in an amount ranging from 0.5% to 2% of the total weight of said filling material; - comprising water-insoluble substrate particles and one or more types of water-soluble components, A pouched product, wherein said water insoluble substrate particles are ball-shaped particles constituting at least 65% by dry weight of said fill material, said water insoluble substrate particles having a d50 particle size of 0.25 mm to 2.0 mm.

2. 2. The pouched product of claim 1, wherein the water insoluble substrate particles have a d50 particle size of 0.25 mm to 1.5 mm.

3. 3. The pouched product of claim 2, wherein the water insoluble substrate particles have a d50 particle size of 0.25 mm to 1.0 mm.

4. 4. A pouched product according to claim 3, wherein the water insoluble substrate particles have a d50 particle size of 0.25mm to 0.6mm, preferably 0.25mm to 0.5mm.

5. 2. The pouched product of claim 1, wherein the water insoluble substrate particles have a d50 particle size of 0.3 mm to 2.0 mm.

6. 6. The pouched product of claim 5, wherein the water insoluble substrate particles have a d50 particle size of 0.3 mm to 1.5 mm.

7. 7. The pouched product of claim 6, wherein the water insoluble substrate particles have a d50 particle size of 0.3 mm to 1.0 mm.

8. 8. A pouched product according to claim 7, wherein the water insoluble substrate particles have a d50 particle size of 0.3 mm to 0.6 mm, preferably 0.3 mm to 0.5 mm.

9. 9. The pouched product of claim 1, wherein the water insoluble substrate particles have a d50 aspect ratio of 0.8 or greater and a d50 sphericity of 0.8 or greater.

10. 10. The pouched product of any one of claims 1 to 9, wherein the water insoluble substrate particles comprise or consist of particles of microcrystalline cellulose, water insoluble starch, silica, or mixtures thereof.

11. 11. The pouched product of claim 10, wherein the water insoluble substrate particles comprise or consist of particles of microcrystalline cellulose.

12. 12. A pouched product according to any one of claims 1 to 11, wherein the water insoluble substrate particles constitute from 75% to 95% by dry weight of the fill material, preferably from 85% to 95% by dry weight of the fill material.

13. 13. The pouched product of any one of claims 1 to 12, wherein the water insoluble substrate particles comprise less than 0.5% by weight of particles passing through a sieve having a mesh size of 250 μm.

14. 14. A pouched product according to any one of the preceding claims, wherein the filling material contains less than 0.5% by weight of particles passing through a sieve having a mesh size of 250 μm.

15. 15. The pouched product of claim 1, wherein the water insoluble substrate particles have a narrow particle size distribution.

16. 16. A pouched product according to any one of claims 1 to 15, wherein the filling material comprises up to 15% sugar alcohol by dry weight of the filling material, preferably up to 10% sugar alcohol by dry weight of the filling material, and most preferably less than 5% sugar alcohol by dry weight of the filling material.

17. 17. The pouched product of claim 1, wherein substantially all of the nicotine in the fill material is disposed on the outer surface of the water-insoluble substrate particles.

18. 18. The pouched product of any one of claims 1 to 17, wherein the liquid-permeable pouch is no more than 80% full.

19. 19. The pouched product of any one of claims 1 to 18, wherein the liquid permeable pouch is formed from a nonwoven material, such as a nonwoven material comprising regenerated cellulose staple fibers.

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