Nicotine composition

Abstract

The present invention describes a composition, e.g., a tobacco-free or low tobacco nicotine-containing composition, comprising: a. nicotine in free base form in an amount of about 0.2% to about 2% by weight; b. natural cellulosic material in an amount of about 35% to about 60% by weight; c. water in an amount of at least 35% by weight; d. one or more pH controlling salts in an amount of about 0.5% to about 3% by weight; e. a release controlling agent comprising agar and / or agar derivatives in an amount of about 0.1% to about 2% by weight; and f. any additional ingredients in an amount preferably up to about 12% by weight. The composition may be provided in a pouch for oral delivery to a user.

Description

Technical Field

[0001] The present invention relates to a tobacco-free or low-tobacco nicotine composition. The composition is preferably for human consumption and can be delivered orally, for example, by placing a permeable pouch filled with the composition into the user's mouth.

Background Art

[0002] A tobacco-free or low-tobacco pouch containing nicotine is an alternative product that can help reduce the cravings associated with smoking tobacco, cigars, or other nicotine delivery products. When tobacco is smoked or when an inhalation-based nicotine delivery system is used, i.e., so-called vaping, nicotine vapor is rapidly absorbed into the bloodstream through the lungs and reaches the brain within 10 seconds after inhalation. The brain produces a near-instantaneous sense of satisfaction, which persists for some time after smoking / inhalation.

[0003] A tobacco-free or low-tobacco pouch containing nicotine is intended to be used in the mouth by placing the pouch under the lip, thereby enabling the release and absorption of nicotine through the oral mucosa. The pouch typically contains a saliva-permeable membrane material and contains other components such as particulate fillers, nicotine or nicotine derivatives, and flavorings. The particulate material may include, among other things, polysaccharides or cellulose materials.

[0004] Nicotine is a type of alkaloid that was traditionally derived from tobacco leaves but may now be provided in a fully synthetic form. It is available both as free base nicotine and in the form of various nicotine salts produced from the interaction of nicotine with acids. Common nicotine salts include chloride, sulfate, benzoate, and tartrate.

[0005] It is known to provide tobacco-free or low-tobacco pouches in which nicotine is provided in the form of a salt in a powder formulation. Providing nicotine salts in such formulations is partly due to the high stability of the system against chemical decomposition and / or evaporation.

[0006] To release free base nicotine from a nicotine salt formulation, the formulation contains a significant amount of buffer salt to increase its alkalinity. As alkalinity increases, the dissociation constant of nicotine changes, resulting in the formation of a free base form from the ionic form of nicotine in the salt in the solution (such as in the user's mouth). Uncharged free base nicotine has higher permeability through the oral mucosa into the bloodstream compared to its ionic form, which is important for consumer use.

[0007] In particular, the pH of nicotine-containing, non-tobacco pouches is typically in the range of 6.9–10.1, with undissociated free base nicotine levels ranging from 7.7–99.2% (Stanfil et al. Nicotine & Tobacco Research, 2021, 1590–1596).

[0008] Therefore, nicotine salt preparations tend to be characterized by a low moisture content, i.e., less than 10% by weight (e.g., 1-8% by weight). This is because a high moisture content promotes the formation of free base nicotine in situ, which reduces product stability because free base nicotine is volatile and unstable to oxidative degradation. When nicotine oxidizes, it turns yellowish-brown, which is often unattractive to consumers and also produces an unpleasant taste. In fact, some preparations contain large amounts of sweeteners (such as maltitol) to stimulate saliva secretion. However, excessive saliva secretion can lead users to spit or swallow, which affects nicotine intake. Furthermore, the degradation of the product exhibits reactivity in the system, which can lead to the presence of undesirable (and potentially toxic) compounds.

[0009] These requirements present problems for users. Formulations with low moisture content can feel hard and unpleasant to the mouth, while high alkalinity (especially above approximately 9 pH) can irritate the user's gums. In contrast, moist nicotine products offer improved palatability when used in the mouth, meaning they are softer and more pleasant.

[0010] Nicotine-containing pouches, including free base nicotine products, are supplied with moisture levels exceeding 35% by weight. However, this type of formulation requires stabilization to prevent nicotine degradation, as well as ingredients to prevent moisture loss during storage. Therefore, wet free base nicotine products tend to require a greater number and quantity of additives than products containing nicotine salts.

[0011] International Publication Nos. 2010 / 104464 and 2010 / 0114445 disclose compositions of free base nicotine that can be stabilized using salts of alginate, such as sodium alginate (e.g., Protanal LFR 5 / 60). The amount of sodium alginate used as a stabilizer is substantial, typically corresponding to a nicotine:Protanal ratio of 1:2 (by weight). International Publication No. 2020244721 discloses a composition of free base nicotine, where the free base nicotine is stabilized using an ion exchange resin, such as a polarilex resin, for example, Amberlite IRP64 (a methacrylic acid polymer containing divinylbenzene, or a potassium salt of divinylbenzene). The amount of polarilex resin used as a nicotine stabilizer is a nicotine-to-resin ratio that can vary between 1:1.19 and 1:4. It should be understood that polymers typically having several carboxylate groups are used to stabilize the free base nicotine.

[0012] To prevent moisture loss during storage of free base nicotine preparations, it is common practice to use humectants such as sugar alcohols. U.S. Patent Application Publication 2020 / 0383372 discloses several compositions of free base nicotine with polarilex resin having a moisture content of more than 15%, most commonly around 30%. Selected humectants include sugar alcohols derived from glycerol, propylene glycol, polyethylene glycol, alginates, pectin, xanthan gum, modified starch, hydroxypropyl cellulose, and triacetin.

[0013] However, the moisture present in the product presents a significant challenge in formulation. Moisture not only acts as a nicotine solvent, facilitating the diffusion of nicotine from the formulation to the oral mucosa, but also as a medium for chemical reactions that can significantly accelerate the rate of chemical decomposition and product spoilage. In fact, nicotine formulations with high moisture content, especially those exceeding 30% by weight, can still be unstable. As mentioned earlier, nicotine decomposition causes discoloration of the product. Furthermore, it is crucial to avoid nicotine decomposition and prevent moisture evaporation during storage. Nicotine decomposition and moisture evaporation can lead to discrepancies between the actual nicotine content and the stated nicotine content (mg of nicotine per gram). This shortens the product's shelf life.

[0014] Physical instability is also a common problem with wet products. Physical instability can include discoloration, stickiness, clumping, and phase transitions (such as dissolution-recrystallization and evaporation). Discoloration and chemical decomposition may be related. If the powder clumps, additional sieving may be required after compounding to control particle size, resulting in additional costs during processing.

[0015] Due to physical and chemical instability, not only may toxic byproducts from nicotine breakdown accumulate, but the product may also have a poor user experience due to color changes (white products turning yellow, brown, or pink), powdering due to drying, leakage from the pouch, hardening of the product, deterioration of mouthfeel, and changes in the nicotine release profile.

[0016] Therefore, there is a need to provide a tobacco-free or low-tobacco nicotine composition that is suitable for use in pouches, has high chemical stability in the nicotine, has high physical stability in the composition, has a pH at a comfortable level for the user, and contains a relatively high moisture content.

[0017] Furthermore, in order to achieve both rapid nicotine release (and thus rapid absorption into the bloodstream) and an improved overall sensory experience for the user, it is necessary to provide nicotine-moistened compositions that are tobacco-free or low in tobacco.

[0018] Furthermore, there is a need to provide such products that can be manufactured in a simple, reliable, and cost-effective manner. [Overview of the project]

[0019] In the first aspect, the present invention is a. Nicotine in the form of free base, approximately 0.2% to 5% by weight, b. Natural cellulose material in an amount of approximately 35% to 60% by weight, c. Water in an amount of at least 35% by weight, d. One or more pH-controlling salts in an amount of approximately 0.5% to approximately 3% by weight, e. A release control agent comprising approximately 0.1% to approximately 2% by weight of agar and / or agar derivatives, f. Preferably containing any additional component in an amount of up to about 12% by weight, The composition is provided. All weight percentages are expressed as a percentage of the total weight of the composition.

[0020] In a second aspect, the present invention provides for the use of agar as a nicotine release control agent in a composition, the composition comprising: a. nicotine in free base form in an amount of from about 0.2% to about 5% by weight; b. a natural cellulose material in an amount of from about 35% to about 60% by weight; c. water in an amount of at least 35% by weight; d. one or more pH control salts in an amount of from about 0.5% to about 3% by weight; e. a release control agent comprising agar in an amount of from about 0.1% to about 2% by weight; f. optionally, additional components in an amount preferably up to about 12% by weight; and comprising.

[0021] In a third aspect, the present invention provides for the use of agar as a nicotine stabilizer in a composition, the composition comprising: a. nicotine in free base form in an amount of from about % to about 5% by weight; b. a natural cellulose material in an amount of from about 35% to about 60% by weight; ​​​​​​​​​​​​​​The sweetener is preferably present in an amount of about 1% to about 3% by weight. The sweetener may comprise a compound selected from saccharides (sucrose, fructose, glucose, dextrose, maltose, lactose, galactose), sugar alcohols (such as xylitol, maltitol, sorbitol, erythritol, etc.) and / or sugar substitutes (such as aspartame, saccharin, sucralose, allulose, acesulfame K, cyclamate or steviol glycoside, etc.).

[0024] Preferably, the sweetener comprises a sugar alcohol in an amount of less than 3% by weight, preferably less than 2% by weight, for example 1% to 2% by weight. Additionally or alternatively, the sweetener may comprise a sugar substitute in an amount of less than 1% by weight, preferably less than 0.5% by weight, for example 0.05% to 0.3% by weight. Preferred sweeteners include xylitol and / or acesulfame K.

[0025] The preservative may comprise one or more preservatives selected from calcium chloride, salts of sorbic acid (such as potassium sorbate), salts of benzoic acid (such as sodium benzoate), nitrates, nitrites, sulfates, sulfites and propionates. Preferably, the preservative is in an amount of less than about 1% by weight, preferably 0.1% to 0.5% by weight, for example about 0.25% to about 0.35% by weight.

[0026] The pH control salt may comprise buffer salts such as carbonates or sesquicarbonates; acetates, glycine salts, acetates, glycine salts, gluconates, borates, glycerophosphates or citrates; phosphates. A combination of ammonium chloride and sodium bicarbonate is preferred. When ammonium chloride is present, its amount may be 0.05% to 1% by weight, preferably 0.1% to 0.5% by weight, for example 0.15% to 0.25% by weight. When sodium bicarbonate is present, its amount may be less than 1% by weight, preferably 0.1% to 0.5% by weight, for example 0.2% to 0.3% by weight.

[0027] Preferably, the composition contains more than 40% by weight of water, for example, 40% to 50% by weight of water, preferably about 44% to about 48% by weight of water.

[0028] Preferably, the natural cellulose material includes powdered cellulose and / or microcrystalline cellulose (MCC), with MCC being preferred.

[0029] The release control agent preferably contains less than about 1% by weight, preferably less than 0.7% by weight, of the composition of agar. In fact, the release control agent may contain about 0.2% to about 0.7% by weight, preferably about 0.2% to about 0.5% by weight, of agar.

[0030] The ratio of agar to nicotine is preferably about 1.3 less than The ratio is 1. In a further preferred embodiment, the agar-to-nicotine ratio is about 0.1:1 to about 1.2:1, preferably about 0.1:1 to about 1:1, and more preferably about 0.1:1 to about 0.8:1.

[0031] Some embodiments may contain tobacco leaves in an amount of less than 5% by weight, preferably about 1% to 3% by weight.

[0032] The pH of the composition, as measured by CORESTA Method No. 69 (2017), is preferably 6 to 9, more preferably 7 to 9, and more preferably 7 to 8.5.

[0033] Preferably, any flavor enhancers present are selected from the group comprising sodium chloride, glutamate, glycine salt, inosinate, and 5'-ribonucleotide salt. If sodium chloride is present, its amount is preferably less than 8% by weight of the composition, preferably 1% to 7% by weight.

[0034] The composition preferably contains less than about 5% by weight of the total composition, for example, less than 3% by weight of the composition, or 0.5% to 3% by weight of the composition, in the form of a flavor compound.

[0035] The preferred amount of nicotine in the composition is 0.2% to 3% by weight, or 0.2% to 2% by weight.

[0036] In some embodiments, the composition may consist essentially of the above-mentioned components.

[0037] In another aspect, the present invention provides a water or saliva-permeable pouch containing the above composition. In yet another aspect, the present invention provides a package containing a plurality of such pouches.

[0038] In a further embodiment, the present invention provides a process for forming the above-described nicotine-containing composition, the process being a. A step of mixing 40% to 60% by weight of natural cellulose material with 0.2% to 2% by weight of agar powder in a mixer to form a precursor composition, b. Add water to the precursor composition and mix at a temperature above 50°C, c. While the temperature is above 50°C, add nicotine in free base form in an amount of 0.2% to about 2% by weight of the target final composition to the precursor composition, d. The step of cooling the mixture, Additional water may be added between steps (c) and (d).

[0039] In a preferred embodiment, the mixing of the precursors in steps (b) and (c) is carried out at a temperature above about 60°C, preferably above about 70°C, and preferably above 80°C.

[0040] In step (b), water may be supplied to the precursor at a temperature above about 70°C, preferably above about 80°C. In fact, in step (b), water may be supplied to the precursor in the form of steam or vapor.

[0041] If additional water is added between step (c) and step (d), the temperature may exceed approximately 70°C, preferably exceeding approximately 80°C. In fact, the additional water may be in the form of steam or vapor.

[0042] In some embodiments, the precursor mixture is heated while in the mixer, for example, during steps (b) and / or (c), and / or during or after any addition of water following step (c).

[0043] In some embodiments, additional water is added to the composition after step (d).

[0044] In a preferred embodiment, any of the following components may be added to the precursor mixture before step (b). e. One or more pH-controlling salts in an amount of approximately 0.5% to approximately 3% by weight of the target composition. f. Preferably, an additional component in an amount of up to about 12% by weight of the target composition.

[0045] Agar is a dry, hydrophilic colloidal polysaccharide complex extracted from red algae (Rhodophyceae). Its structure is thought to consist of various complex polysaccharide chains with alternating α-(1→3) and β-(1→4) bonds. Agar can be separated into agarose, the natural gelling fraction, and agaropectin, the sulfated non-gelling fraction. Agar dissolves in hot water to form a viscous solution, but is sparingly soluble in cold water and ethanol (95%). A 1 wt / vol% aqueous solution forms a firm jelly when cooled.

[0046] When the term "tobacco" is used, it refers to any part of any member of the genus Nicotiana (such as leaves, stems, and stalks). Tobacco may be whole, shredded, hulled, cut, crushed, hardened, aged, fermented, or otherwise processed (e.g., granulated or encapsulated).

[0047] Herein, embodiments of the present invention will be described with reference to the following drawings. [Brief explanation of the drawing]

[0048] [Figure 1] This figure shows plots of the nicotine release profiles of compositions according to the present invention and comparative examples. [Figure 2] This figure shows plots of the nicotine release profiles of compositions according to the present invention and comparative examples. [Figure 3] This figure shows photographs of pouches and compositions according to the present invention and comparative examples. [Modes for carrying out the invention]

[0049] In a first embodiment of the present invention, a tobacco-free (or optionally low-tobacco) nicotine preparation for use in an oral pouch is provided. The preparation has a high water content and contains nicotine in the form of its free base. The composition comprises a cellulose-based filler, and agar is used as a nicotine release agent to facilitate the release of nicotine from the composition when the composition is placed in the user's mouth (for example, in a pouch).

[0050] In one embodiment, the composition has a general formulation as described below. a. Nicotine in free base form, approximately 0.2% to 5% by weight. b. Natural cellulose material in an amount of approximately 35% to 60% by weight, for example, microcrystalline cellulose. c. Water in an amount of at least 35% by weight, d. One or more pH-controlling salts in an amount of approximately 1% to 6% by weight, for example, a combination of ammonium chloride and sodium bicarbonate. e. A release control agent containing approximately 0.1% to 2% by weight of agar or its derivative. f. Preferably, any additional ingredients in an amount of up to about 12% by weight, such as flavorings, flavor enhancers, sweeteners, and preservatives.

[0051] All weight percentages are based on the total weight of the composition.

[0052] The amount of nicotine in the composition varies depending on the desired strength of the product. In some embodiments, the amount of nicotine is 0.2% to 3% by weight, or 0.2% to 2% by weight.

[0053] Natural cellulose useful in the present invention may include powdered cellulose and / or microcrystalline cellulose. Examples of powdered cellulose that can be used in the present invention include Arbocel (RTM), Elcema supplied by J. Rettenmaier & Soehne GmbH, KC Flock (RTM), supplied by Nippon Paper Industries Co. Ltd., Microcel 3E-150, supplied by Roquette Freres, Sanacel (RTM), supplied by CFF GmbH, Sanacel Pharma (RTM), supplied by CFF GmbH, Sancel-W, supplied by NB Entrepreneurs Company, or Solka-Floc (RTM), supplied by J. Rettenmaier USA LP.

[0054] Examples of microcrystalline cellulose that can be used in the present invention include Avicel(RTM)PH supplied by Dupont Nutrition and Biosciences, Inc., Cellets(RTM) supplied by Pharmatrans Sanaq AG, Celphere(TM) supplied by Asahi Kasei Corporation, Ceolus(TM)KG supplied by Asahi Kasei Corporation, Emcocel(RTM) supplied by JRS Pharma GmbH, MCC Sanaq(RTM) supplied by Pharmatrans Sanaq AG, Pharmacel(RTM) supplied by DFE Pharma GmbH, Tabulose(RTM) supplied by Roquette Freres, and Vivapur(RTM) supplied by JRS Pharma GmbH.

[0055] The composition must have a water content of at least 35% by weight, but a higher proportion of water is preferable. When the water content of the composition exceeds 40% by weight, the palatability for the user tends to improve, such as increased softness. Preferred compositions have a water content exceeding 42% by weight, for example, 44% to 48% by weight of water.

[0056] The composition contains a pH-controlling salt to provide an optimal pH for use in the user's mouth. The pH of the composition is preferably 6–9, preferably 7–9, and more preferably 7–8.5, as measured according to CORESTA Method No. 69 (2017). This can be achieved by providing a pH adjuster such as sodium bicarbonate, or a buffer salt such as a combination of ammonium chloride and sodium bicarbonate. A typical amount of the pH-controlling salt is 0.2%–2% by weight, preferably 0.2%–1% by weight. Alternative buffer salts may be selected from, for example, carbonates or sesquicarbonates; acetates, glycinates, glucons, borates, glycerophosphates or citrates; and phosphates.

[0057] The flavorings included in the composition are not limited, but preferably include flavonoid compounds that stimulate the user's olfactory system, typically in an amount of less than about 3% by weight of the total composition. Such compounds are commercially available and well known to those skilled in the art.

[0058] The flavor of the composition can be improved by including sweeteners or flavor enhancers.

[0059] Examples of sweeteners include sugar-based sweeteners such as sucrose, fructose, glucose, dextrose, maltose, lactose, and galactose; sugar alcohols such as xylitol, maltitol, sorbitol, and erythritol; or other sugar substitutes such as aspartame, saccharin, sucralose, allulose, acesulfame K, cyclamate, or steviol glycosides. Sweeteners may exist alone, but are preferably used in combination (e.g., sugar alcohols and sugar substitutes). A preferred combination is xylitol and acesulfame K. The amount of sweetener present in the composition depends on the properties of the selected sweetener, as will be understood by those skilled in the art, but is typically in the range of 1% to 3% by weight in total.

[0060] Flavor enhancers may include sodium chloride, glutamic acid salts (such as monosodium glutamate), glycine salts, inosinates, and 5'-ribonucleotide salts (such as one or more disodium ribonucleotides). The amount of flavor enhancers present in the composition depends on the properties of the selected flavor enhancers, as will be understood by those skilled in the art, but is typically in the range of 1% to 8% by weight in total.

[0061] Preservatives may include antimicrobial preservatives such as sorbates (sodium sorbate or potassium sorbate, etc.), benzoates, nitrates, nitrites, sulfates, sulfites, and propionates. Salts such as calcium chloride can also be used as preservatives.

[0062] All compositions may contain small amounts of tobacco, such as 1% to 5% by weight, especially when packaged in pouches.

[0063] The inventors have surprisingly found that the presence of agar in the composition acts as an effective nicotine stabilizer and release controller. While we do not wish to be bound by any particular theory, it is hypothesized that nicotine may be partially bound within the agar gel that may be formed during manufacturing. This appears to provide a highly stable nicotine composition that can be stored for long periods, despite the use of free base nicotine and high levels of water. Furthermore, the nicotine release profile of the composition is fast and consistent, providing excellent product performance.

[0064] This performance is achieved even though only a relatively small amount of agar is provided in the composition. The agar is preferably present in an amount of 0.1% to about 1.2% by weight. Preferably, the agar-to-nicotine ratio is about 0.1:1 to about 1.2:1, preferably about 0.1:1 to about 1:1, and more preferably about 0.1:1 to about 0.8:1. This is a significantly lower ratio than that required for conventional stabilizers.

[0065] In this invention, any food or pharmaceutical grade agar can be used. Specific examples include Rokoagar (RTM) RGM 600 and RGM 800 supplied by Industrias Roko, SA.

[0066] In preferred embodiments, the composition may have the following general composition: a. Nicotine in free base form, approximately 0.2% to 3% by weight. b. Microcrystalline cellulose in an amount of approximately 35% to 60% by weight. c. Water in an amount of at least 35% by weight, preferably more than 40% by weight, d. 0.05% and 1% by weight of ammonium chloride and approximately 0.1% to approximately 1% by weight of sodium bicarbonate buffer salt, e. A release control agent containing approximately 0.1% to 2% by weight of agar. f. Any additional components, for example. a. Flavorings in an amount of 0.5% to approximately 3% by weight. b. Flavor enhancers such as sodium chloride in an amount of 2% to 8% by weight. c. Approximately 1% to 2% by weight of xylitol and / or 0.05% to 1% by weight of a sweetener such as acesulfame K. d. A preservative such as potassium sorbate in an amount of approximately 0.25% to 1% by weight. e. Tobacco in an amount of 0% to 3% by weight.

[0067] In further embodiments, a process is provided for producing tobacco-free or low-tobacco nicotine compositions. This process involves mixing, in a container (such as an autoclave), 30% to 60% by weight of natural cellulose and 0.1% to 2% by weight of agar, each in powder or granular form, of the desired final composition. One or more other solid components of the composition (e.g., pH-controlling salts, flavor enhancers, sweeteners, or preservatives) can also be added at this stage of the process, but any tobacco intended to be included in the final composition should ideally be retained until the rest of the composition is complete.

[0068] Next, at least a portion of water (preferably at least 10% by weight of the target final composition) is added to the composition, and the composition is heated. Heating can be carried out in various ways. The mixing vessel may be heated, for example, using a heating manifold. Alternatively or additionally, the water may be heated before being introduced into the mixing vessel, or some or all of the water may be added as steam.

[0069] The temperature of the resulting precursor mixture must be at least 50°C, preferably at least 60°C, and more preferably at least 70°C. The precursor is heated so that the agar dissolves at least partially in water. While we do not wish to be bound by any theory, it is assumed that the low concentration of agar, combined with the shear force applied during mixing, may cause the agar to dissolve sufficiently at such temperatures.

[0070] While the heated precursor mixture is being mixed, nicotine is added to the precursor in an amount of 0.2% to 2% by weight of the final composition. At this stage, other liquid components of the composition, such as flavorings, may be added.

[0071] Optionally, the second portion of water (preferably at least 10% by weight of the target final composition) is then added to the composition, and the composition is heated again to at least 50°C, preferably at least 60°C, and more preferably 70°C.

[0072] Next, the precursor is cooled, preferably while continuing to mix. The resulting composition may be set aside. While we do not wish to be bound by any particular theory, it is thought that agar forms a gel that at least partially encapsulates the present nicotine, stabilizing it and providing excellent release properties.

[0073] In any finishing step, water may be added to the resulting composition (preferably at room temperature). This step is to provide the composition with a higher content as needed. In some embodiments, flavor enhancers, sweeteners, or preservatives may be added at this stage in addition to, or instead of, an earlier stage of the process.

[0074] The finished composition can optionally be mixed with tobacco in an amount up to 5% by weight of the final composition. This composition is soft to the touch, virtually dust-free, and does not form clumps. The product is white. In a preferred embodiment, it is packaged in a saliva-permeable pouch for oral delivery. [Examples]

[0075] Various compositions were prepared according to the method described above. [Table 1]

[0076] Each 0.7g portion of the completed composition was placed in a saliva-permeable pouch and tested according to the following release test.

[0077] One participant will avoid nicotine intake for 10 hours prior to the start of the experiment and avoid consuming food or drink for 1 hour prior to the start of the experiment. Before the procedure, the participant will rinse their mouth with water and wait for 10 minutes.

[0078] Take the pouch, weigh it, and place it under the subject's lips. Leave the pouch undisturbed for 5 minutes. Next, remove the pouch and measure 50 cm. 3 Place in distilled water and stir or shake for 30 minutes. Take a sample and analyze the nicotine content using HPLC.

[0079] The tester then waits at least one hour before repeating the experiment, holding the pouch in place for 10, 20, 30, and 40 minutes in a series of repetitions.

[0080] The results of the release test are shown in Figure 1. As can be seen from the figure, the inclusion of 20% by weight of agar slightly increases both the nicotine release rate and the total amount released over 40 minutes. However, surprisingly, when the proportion of agar in the composition is relatively low (0.3% by weight, 0.6% by weight of nicotine), both the release rate and the total amount released over 40 minutes increase significantly.

[0081] Further compositions identical to those in Example 1, but containing a different stabilizer instead of agar, were prepared and tested according to the same method. The stabilizers used in these examples are shown in the table below. [Table 2]

[0082] The results of the release test are shown in the graph in Figure 2, overlaid with the plot from Example 1. From the plot, it is clear that in the case of agar, the total amount of nicotine released is greatest over 40 minutes, and that nicotine release is significantly faster in the first 10 minutes after starting use. This is a great advantage for users who are trying to quit smoking.

[0083] pH test - CORESTA method No. 69 (2017) Calibrate the pH electrode using at least two pH buffer solutions (4.00 and 7.00 or 7.00 and 10.00) to perform a two-point calibration covering the pH range of the product under test. Calibration should be performed at 23°C along with the sample measurement. The calibration gradient must be within 95%–105% before the electrode is ready for sample measurement. The electrode must be rinsed with water before and after each measurement.

[0084] Allow the test sample to reach room temperature before preparation. Next, mix the sample with water to a concentration of 5% by weight and shake or stir for 30 minutes. Then, measure the pH of the water in the sample mixture using a pH electrode.

[0085] Comparative Examples 10-12 Comparative Examples 10-12 list commercially available products based on nicotine salts and characterized by low moisture content, i.e., less than 10% by weight. These products generally feature a long shelf life of at least 12 months. However, discoloration and clumping increase with increasing moisture content. Very dry products may become powdery during storage and become difficult to handle during packaging. Low-moisture products are typically characterized by poor palatability (dry mouthfeel) and delayed nicotine release. The appearance of the samples is shown in Figure 3. [Table 3] [Table 4] [Table 5]

[0086] Comparative Examples 13-17 Comparative Examples 13–17 list commercially available products based on nicotine free base and characterized by a high moisture content, i.e., over 40% by weight. Almost all products are characterized by lumping and varying degrees of discoloration. Comparative Examples 13–16 are variations of the same product from the same manufacturer, differing primarily in the flavorings, release regulators, and sweeteners used. The products in these examples contain calcium chloride. Calcium chloride is typically used as an excipient with water-binding properties and as an antimicrobial preservative. The appearance of the samples is shown in Figure 3. [Table 6] [Table 7] [Table 8] [Table 9] [Table 10]

[0087] Comparative Examples 18 and 19 Comparative Examples 18 and 19 list commercially available products based on free base nicotine and characterized by a moderate moisture content, i.e., less than 10–30% by weight. These products are characterized by a shelf life of approximately 6–12 months. Both products show signs of discoloration and lumping. Comparative Example 16, which contains a high amount of sugar alcohol, is particularly prone to lumping and hardens over time, significantly reducing the palatability of the product. The appearance of the samples is shown in Figure 3. [Table 11] [Table 12]

[0088] Example 2 Example 2 illustrates an example of a formulation according to the present invention. This product is characterized by a high moisture content and high nicotine stability during storage for at least 12 months. After storage, no signs of discoloration, clumping, or powdering are observed. [Table 13]

[0089] The examples demonstrate that the composition of the present invention provides a soft, white product that avoids clumping, is therefore pleasant to the mouth during use, and is easy to package and manufacture. Furthermore, it has a long shelf life and delivers nicotine to the user quickly and consistently.

[0090] The present invention relates to the following: It encompasses various aspects. [Aspect 1] A composition, a. Nicotine in the form of free base, approximately 0.2% to 5% by weight, b. Natural cellulose material in an amount of approximately 35% to 60% by weight, c. Water in an amount of at least 35% by weight, d. One or more pH-controlling salts in an amount of approximately 0.5% to approximately 3% by weight, e. A release control agent comprising approximately 0.1% to approximately 2% by weight of agar and / or agar derivatives, f. Preferably, any additional component in an amount of up to about 12% by weight. A composition containing the following: [Aspect 2] The composition according to embodiment 1, further comprising, preferably, an additional component in an amount of about 1% to about 10% by weight, or more preferably, about 1% to about 8% by weight. [Aspect 3] The composition according to Embodiment 1 or Embodiment 2, wherein the additional component comprises one or more additives selected from flavorings, flavor enhancers, sweeteners, and preservatives. [Aspect 4] The composition according to embodiment 2 or 3, wherein the additional component preferably contains a sweetener in an amount of about 1% to about 3% by weight. [Aspect 5] The composition according to embodiment 4, wherein the sweetener comprises a compound selected from sugars (sucrose, fructose, glucose, dextrose, maltose, lactose, galactose), sugar alcohols (xylitol, maltitol, sorbitol, erythritol, etc.) and / or sugar substitutes (aspartame, saccharin, sucralose, allulose, acesulfame K, cyclamate, or steviol glycosides, etc.). [Aspect 6] The composition according to embodiment 4 or 5, comprising less than 3% by weight, preferably less than 2% by weight, for example, 1% to 2% by weight of sugar alcohol. [Aspect 7] The composition according to any one of embodiments 4 to 6, comprising less than 1% by weight, preferably less than 0.5% by weight, for example, 0.05% to 0.3% by weight of a sugar substitute. [Aspect 8] The composition according to embodiment 6 or 7, wherein the sugar alcohol comprises xylitol and / or the sugar substitute comprises acesulfame K. [Aspect 9] The composition according to any one of embodiments 2 to 8, further comprising one or more preservatives selected from calcium chloride, sorbic acid salts (such as potassium sorbate), benzoic acid salts (such as sodium benzoate), nitrates, nitrites, sulfates, sulfites, and propionates. [Aspect 10] The composition according to embodiment 9, wherein potassium sorbate is present in an amount of less than about 1% by weight, preferably 0.1% to 0.5% by weight, for example, about 0.25% to about 0.35% by weight. [Aspect 11] The composition according to any one of embodiments 1 to 9, wherein the pH control salt includes a buffer salt such as a combination of ammonium chloride and sodium bicarbonate. [Aspect 12] The composition according to embodiment 11, wherein ammonium chloride is present in an amount of 0.05% to 1% by weight, preferably 0.1% to 0.5% by weight, for example, 0.15% to 0.25% by weight. [Aspect 13] The composition according to any one of embodiments 1 to 12, wherein sodium bicarbonate is present in an amount of less than 1% by weight, preferably 0.1% to 0.5% by weight, for example, 0.2% to 0.3% by weight. [Aspect 14] The composition according to any one of embodiments 1 to 13, comprising more than 40% by weight of water, for example, 40% to 50% by weight of water, preferably about 44% to about 48% by weight of water. [Aspect 15] The composition according to any one of embodiments 1 to 14, wherein the filler comprises powdered cellulose and / or microcrystalline cellulose (MCC). [Aspect 16] The composition according to any one of embodiments 1 to 15, wherein the release control agent contains an amount of agar less than about 1% by weight, preferably less than 0.7% by weight. [Aspect 17] The composition according to embodiment 16, wherein the release control agent contains agar in an amount of about 0.2% to about 0.7% by weight, preferably about 0.2% to about 0.5% by weight. [Aspect 18] The composition according to any one of embodiments 1 to 17, wherein the agar-to-nicotine ratio is less than approximately 1.3:1. [Aspect 19] The composition according to any one of embodiments 1 to 18, wherein the agar-to-nicotine ratio is about 0.1:1 to about 1.2:1, preferably about 0.1:1 to about 1:1, and more preferably about 0.1:1 to about 0.8:1. [Aspect 20] The composition according to any one of embodiments 1 to 19, further comprising less than 5% by weight, preferably about 1% to 3% by weight, of tobacco leaves. [Aspect 21] The composition according to any one of embodiments 1 to 20, wherein the pH measured by CORESTA method No. 69 (2017) is 6 to 9, preferably 7 to 9, and more preferably 7 to 8.5. [Aspect 22] The composition according to any one of embodiments 3 to 21, wherein the flavor enhancer is selected from the group comprising sodium chloride, glutamate, glycine salt, inosinate, and 5'-ribonucleotide salt. [Aspect 23] The composition according to embodiment 22, comprising less than 8% by weight, preferably 1% to 7% by weight, of sodium chloride. [Aspect 24] The composition according to any one of embodiments 3 to 23, comprising a flavor compound in an amount of less than approximately 5% by weight of the total composition, for example, less than 3% by weight of the composition, or 0.5% to 3% by weight of the composition. [Pattern 25] The composition according to any one of embodiments 1 to 24, wherein the amount of nicotine is 0.2% to 3% by weight, or 0.2% to 2% by weight. [Aspect 26] A composition according to any one of embodiments 1 to 25, which essentially consists of the components described in the embodiment. [Aspect 27] A water or saliva-permeable pouch comprising the composition described in any one of embodiments 1 to 26. [Aspect 28] A package comprising multiple pouches as described in Embodiment 27. [Aspect 29] A process for forming a nicotine-containing composition according to any one of embodiments 1 to 26. a. A step of mixing 40% to 60% by weight of natural cellulose material of the target composition with 0.2% to 2% by weight of agar (and / or agar derivative) powder in a mixer to form a precursor composition, b. Adding water to the precursor composition and mixing at a temperature above 50°C, c. While the temperature is above 50°C, add nicotine in free base form in an amount of 0.2% to about 2% by weight of the target final composition to the precursor composition; d. A step of cooling the mixture, A process that includes this. [Aspect 30] The process according to embodiment 29, wherein additional water is added between step (c) and step (d). [Aspect 31] The process according to embodiment 29 or 30, wherein in steps (b) and (c), the mixing of the precursors is carried out at a temperature above about 60°C, preferably above about 70°C, preferably above 80°C. [Aspect 32] The process according to any one of embodiments 29 to 31, wherein in step (b), the water is supplied to the precursor at a temperature exceeding approximately 70°C, preferably exceeding approximately 80°C. [Aspect 33] The process according to embodiment 32, wherein in step (b), the water is supplied to the precursor in the form of steam or vapor. [Aspect 34] The process according to any one of embodiments 30 to 33, wherein the temperature of the additional water added between step (c) and step (d) exceeds approximately 70°C, preferably exceeding approximately 80°C. [Aspect 35] The process according to embodiment 34, wherein the additional water added between step (c) and step (d) is in the form of steam or vapor. [Aspect 36] The process according to any one of embodiments 29 to 35, wherein the precursor mixture is heated while in the mixer, for example, during step (b) and / or (c), and / or during or after any addition of water following step (c). [Aspect 37] The process according to any one of embodiments 29 to 36, wherein further water is added to the composition after step (d). [Aspect 38] Before step (b), add the following ingredients: a. One or more pH-controlling salts in an amount of about 0.5% to about 3% by weight of the target composition. b. Preferably an additional component in an amount of up to about 12% by weight of the target composition. The process according to any one of embodiments 29 to 37, wherein one of the above is added to the precursor mixture. [Aspect 39] The process according to any one of embodiments 29 to 38, wherein the target composition is the composition according to any one of embodiments 1 to 26. [Aspect 40] a. Nicotine in the form of free base, approximately 0.2% to 5% by weight, b. Natural cellulose material in an amount of approximately 35% to 60% by weight, c. Water in an amount of at least 35% by weight, d. One or more pH-controlling salts in an amount of approximately 0.5% to approximately 3% by weight, e. A release control agent comprising approximately 0.1% to approximately 2% by weight of agar and / or agar derivatives, f. Preferably, any additional component in an amount of up to about 12% by weight. Use of agar as a nicotine release control agent in compositions containing [the specified substance]. [Aspect 41] a. Nicotine in the form of free base, approximately 0.2% to 5% by weight, b. Natural cellulose material in an amount of approximately 35% to 60% by weight, c. Water in an amount of at least 35% by weight, d. One or more pH-controlling salts in an amount of approximately 0.5% to approximately 3% by weight, e. A release control agent comprising approximately 0.1% to approximately 2% by weight of agar and / or agar derivatives, f. Preferably, any additional component in an amount of up to about 12% by weight. Use of agar as a nicotine stabilizer in compositions containing [the specified substance]. [Aspect 42] The use according to embodiment 38 or embodiment 39, wherein the composition further comprises an additional component preferably in an amount of about 1% to about 10% by weight, or more preferably in an amount of about 1% to about 8% by weight. [Aspect 43] The use according to any one of embodiments 40 to 42, wherein the additional component in the composition comprises one or more additives selected from flavorings, flavor enhancers, sweeteners, and preservatives. [Aspect 44] The use according to embodiment 42 or embodiment 43, wherein the additional component preferably contains a sweetener in an amount of about 1% to about 3% by weight. [Aspect 45] The use according to embodiment 44, wherein the sweetener comprises a compound selected from sugars (sucrose, fructose, glucose, dextrose, maltose, lactose, galactose), sugar alcohols (xylitol, maltitol, sorbitol, erythritol, etc.) and / or sugar substitutes (aspartame, saccharin, sucralose, allulose, acesulfame K, cyclamate, or steviol glycosides, etc.). [Aspect 46] The use according to embodiment 44 or embodiment 45, comprising less than 3% by weight, preferably less than 2% by weight, for example, 1% to 2% by weight of sugar alcohol. [Aspect 47] The use according to embodiment 46, comprising less than 1% by weight, preferably less than 0.5% by weight, for example, 0.05% to 0.3% by weight of the sugar substitute. [Aspect 48] The use according to embodiment 46 or embodiment 47, wherein the sugar alcohol comprises xylitol and / or the sugar substitute comprises acesulfame K. [Aspect 49] The use according to any one of embodiments 42 to 48, further comprising one or more preservatives selected from calcium chloride, sorbic acid salts (such as potassium sorbate), benzoic acid salts (such as sodium benzoate), nitrates, nitrites, sulfates, sulfites, and propionates. [Aspect 50] The use according to embodiment 49, wherein potassium sorbate is present in an amount of less than about 1% by weight, preferably 0.1% to 0.5% by weight, for example, about 0.25% to about 0.35% by weight. [Aspect 51] The use according to any one of embodiments 40 to 49, wherein the pH control salt includes a buffer salt such as a combination of ammonium chloride and sodium bicarbonate. [Aspect 52] The use according to embodiment 51, wherein ammonium chloride is present in an amount of 0.05% to 1% by weight, preferably 0.1% to 0.5% by weight, for example, 0.15% to 0.25% by weight. [Aspect 53] The use according to any one of embodiments 40 to 52, wherein sodium bicarbonate is present in an amount of less than 1% by weight, preferably 0.1% to 0.5% by weight, for example, 0.2% to 0.3% by weight. [Aspect 54] The use according to any one of embodiments 40 to 53, comprising more than 40% by weight of water, for example, 40% to 50% by weight of water, preferably about 44% to about 48% by weight of water. [Aspect 55] The use according to any one of embodiments 40 to 54, wherein the filler comprises powdered cellulose and / or microcrystalline cellulose (MCC). [Aspect 56] The use according to any one of embodiments 40 to 55, wherein the release control agent contains an amount of agar in less than about 1% by weight, preferably less than 0.7% by weight. [Aspect 57] The use according to embodiment 56, wherein the release control agent contains agar in an amount of about 0.2% to about 0.7% by weight, preferably about 0.2% to about 0.5% by weight. [Aspect 58] The use according to any one of embodiments 40 to 57, wherein the agar-to-nicotine ratio is less than approximately 1.3:1. [Aspect 59] The use according to any one of embodiments 40 to 58, wherein the agar-to-nicotine ratio is approximately 0.1:1 to approximately 1.2:1, preferably approximately 0.1:1 to approximately 1:1, and more preferably approximately 0.1:1 to approximately 0.8:1. [Aspect 60] The use according to any one of embodiments 40 to 59, further comprising an amount of tobacco leaves less than 5% by weight, preferably about 1% to 3% by weight. [Aspect 61] The use according to any one of embodiments 40 to 60, wherein the pH measured by CORESTA method No. 69 (2017) is 6 to 9, preferably 7 to 9, and more preferably 7 to 8.5. [Aspect 62] The use according to any one of embodiments 43 to 61, wherein the flavor enhancer is selected from the group comprising sodium chloride, glutamate, glycine salt, inosinate, and 5'-ribonucleotide salt. [Aspect 63] The use according to embodiment 62, comprising less than 8% by weight, preferably 1% to 7% by weight of sodium chloride. [Aspect 64] The use according to any one of embodiments 43 to 63, comprising a flavor compound in an amount less than approximately 5% by weight of the total composition, for example, less than 3% by weight of the composition, or 0.5% to 3% by weight of the composition. [Aspect 65] The use according to any one of embodiments 40 to 64, wherein the amount of nicotine is 0.2% to 3% by weight, or 0.2% to 2% by weight. [Aspect 66] The use according to any one of embodiments 40 to 65, wherein the composition essentially consists of the components described in the embodiments.

Claims

1. a. Nicotine in the form of free base, at a concentration of 0.2% to 5% by weight b. Natural cellulose material in an amount of 35% to 60% by weight, c. Water in an amount of at least 35% by weight, d. One or more pH-controlling salts in an amount of 0.5% to 3% by weight, e. A release control agent comprising 0.1% to 2% by weight of agar and / or an agar derivative, Use of agar as a nicotine release control agent in a composition containing the following, where the weight ratio of agar to nicotine is 0.1:1 to 1.2:

1.

2. a. Nicotine in the form of free base, at a concentration of 0.2% to 5% by weight b. Natural cellulose material in an amount of 35% to 60% by weight, c. Water in an amount of at least 35% by weight, d. One or more pH-controlling salts in an amount of 0.5% to 3% by weight, e. A release control agent comprising 0.1% to 2% by weight of agar and / or an agar derivative, The use of agar as a nicotine stabilizer in a composition containing the following, where the weight ratio of agar to nicotine is 0.1:1 to 1.2:

1.

3. The use according to claim 1 or claim 2, wherein the composition further comprises additional components.

4. The use according to claim 3, wherein the composition comprises an additional component in an amount of up to 12% by weight.

5. The use according to claim 3 or claim 4, wherein the additional component in the composition comprises one or more additives selected from flavorings, flavor enhancers, sweeteners, and preservatives.

6. The use according to any one of claims 3 to 5, wherein the additional component includes a sweetener.

7. The use according to claim 6, wherein the sweetener is present in an amount of 1% to 3% by weight.

8. The use according to claim 6 or 7, wherein the sweetener comprises a compound selected from sugars, sugar alcohols and / or sugar substitutes.

9. The use according to claim 8, wherein the sugars are sucrose, fructose, glucose, dextrose, maltose, lactose, or galactose, the sugar alcohol is xylitol, maltitol, sorbitol, or erythritol, and / or the sugar substitute is aspartame, saccharin, sucralose, allulose, acesulfame K, cyclamate, or steviol glycosides.

10. The use according to any one of claims 6 to 9, comprising less than 3% by weight of a sugar alcohol.

11. The use according to any one of claims 6 to 10, comprising less than 1% by weight of the sugar substitute.

12. The use according to claim 10 or claim 11, wherein the sugar alcohol comprises xylitol and / or the sugar substitute comprises acesulfame K.

13. The use according to any one of claims 3 to 12, further comprising one or more preservatives selected from calcium chloride, salts of sorbic acid, salts of benzoic acid, nitrates, nitrites, sulfates, sulfites, and propionates.

14. The use according to claim 13, wherein the salt of sorbic acid is potassium sorbate and / or the salt of benzoic acid is sodium benzoate.

15. The use according to claim 13 or 14, wherein potassium sorbate is present in an amount of less than 1% by weight.

16. The use according to any one of claims 1 to 14, wherein the pH control salt includes a buffer salt.

17. The use according to claim 16, wherein the buffer salt is a combination of ammonium chloride and sodium bicarbonate.

18. The use according to claim 16 or 17, wherein ammonium chloride is present in an amount of 0.05% to 1% by weight.

19. The use according to any one of claims 1 to 18, wherein sodium bicarbonate is present in an amount of less than 1% by weight.

20. The use according to any one of claims 1 to 19, comprising more than 40% by weight of water.

21. The use according to any one of claims 1 to 20, wherein the natural cellulose material comprises powdered cellulose and / or microcrystalline cellulose (MCC).

22. The use according to any one of claims 1 to 21, wherein the release control agent contains an amount of less than 1% by weight of agar.

23. The use according to claim 22, wherein the release control agent contains agar in an amount of 0.2% to 0.7% by weight.

24. The use according to any one of claims 1 to 23, further comprising less than 5% by weight of tobacco leaves.

25. The use according to any one of claims 1 to 24, wherein the pH measured by the CORESTA method No. 69 (2017) is between 6 and 9.

26. The use according to any one of claims 5 to 25, wherein the flavor enhancer is selected from the group comprising sodium chloride, glutamate, glycine salt, inosinate, and 5'-ribonucleotide salt.

27. The use according to claim 26, comprising less than 8% by weight of sodium chloride.

28. The use according to any one of claims 5 to 27, comprising a flavor compound in an amount of less than 5% by weight of the total composition.

29. The use according to any one of claims 1 to 28, wherein the amount of nicotine is 0.2% to 3% by weight, or 0.2% to 2% by weight.

30. The use according to any one of claims 1 to 29, wherein the composition essentially consists of the components described in any one of claims 1 to 29.

31. A process for forming a nicotine-containing composition, wherein the process is a. A step of mixing 40% to 60% by weight of natural cellulose material of the target composition with 0.2% to 2% by weight of agar (and / or agar derivative) powder of the target composition in a mixer to form a precursor composition, b. A step of adding water to the precursor composition and mixing at a temperature above 50°C, c. While the temperature is above 50°C, add nicotine in free base form in an amount of 0.2% to 2% by weight of the target final composition to the precursor composition; d. A step of cooling the mixture, Includes, The aforementioned target composition is a. Nicotine in the form of free base, at a concentration of 0.2% to 5% by weight b. Natural cellulose material in an amount of 35% to 60% by weight, c. Water in an amount of at least 35% by weight, d. One or more pH-controlling salts in an amount of 0.5% to 3% by weight, e. A release control agent comprising 0.1% to 2% by weight of agar and / or an agar derivative, A process comprising a composition having a weight ratio of agar to nicotine of 0.1:1 to 1.2:

1.

32. The process according to claim 31, wherein additional water is added between step (c) and step (d).

33. The process according to claim 31 or 32, wherein in steps (b) and (c), the mixing of the precursors is carried out at a temperature above 60°C.

34. The process according to any one of claims 31 to 33, wherein in step (b), the water is supplied to the precursor at a temperature exceeding 70°C.

35. The process according to claim 34, wherein in step (b), the water is supplied to the precursor in the form of steam or vapor.

36. The process according to any one of claims 32 to 35, wherein the temperature of the additional water added between step (c) and step (d) exceeds 70°C.

37. The process according to claim 36, wherein the additional water added between step (c) and step (d) is in the form of steam or vapor.

38. The process according to any one of claims 31 to 37, wherein the precursor mixture is heated while it is in the mixer.

39. The process according to claim 38, wherein the precursor mixture is heated while in the mixer during steps (b) and / or (c), and / or during or after any addition of water following step (c).

40. The process according to any one of claims 31 to 39, wherein further water is added to the composition after step (d).

41. Before step (b), add the following ingredients: a. One or more pH-controlling salts in an amount of 0.5% to 3% by weight of the target composition. b. The process according to any one of claims 31 to 40, wherein one of the additional components is added to the precursor mixture.

42. The process according to claim 41, wherein the additional component is added in an amount up to 12% by weight of the target composition.

43. The process according to any one of claims 31 to 42, wherein the target composition is the composition according to any one of claims 1 to 30.

44. A composition, a. Nicotine in the form of free base, at a concentration of 0.2% to 5% by weight b. Natural cellulose material in an amount of 35% to 60% by weight, c. Water in an amount of at least 35% by weight, d. One or more pH-controlling salts in an amount of 0.5% to 3% by weight, e. A release control agent comprising 0.5% to 2% by weight of agar and / or an agar derivative, A composition comprising agar to nicotine in a weight ratio of 0.1:1 to 1.2:

1.

45. The composition according to claim 44, wherein the composition is one of those described in any one of claims 1 to 30.

46. The composition according to claim 44 or 45, wherein the release control agent comprises 0.7% to 2% by weight of agar.

47. A water or saliva-permeable pouch comprising the composition according to any one of claims 44 to 46.

48. A package comprising a plurality of pouches as described in claim 47.

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