PAPER SHEET COMPRISING A PLANT EXTRACT AND STABILIZED NICOTINE
Patent Information
- Application Number
- FR2024001604
- Authority / Receiving Office
- FR · FR
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2024-02-19
- Publication Date
- 2025-08-22
Abstract
Description
Title of the invention: SHEET OF PAPER COMPRISING A PLANT EXTRACT AND STABILIZED NICOTINE Technical field
[0001] The present disclosure belongs to the field of devices for heating tobacco without burning it and relates to a sheet of paper comprising stabilized nicotine. Prior art
[0002] In recent years, a large number of devices have been developed to provide nicotine to a user while avoiding the formation of harmful components during the combustion of tobacco. These devices are, for example, the E-cigarette and devices for heating tobacco without burning it.
[0003] E-cigarettes generate a nicotine-containing aerosol by heating a solution of nicotine / nicotine salt and aerosol-generating agent contained in a cartridge of said E-cigarette. The solution may also include flavorings. E-cigarettes offer a wide range of strengths and tastes by modulating the concentration of nicotine salts and varying the nature and quantity of flavorings. However, it can be difficult to introduce the solution into the cartridge and the cartridge can leak during use. Not only can the user get their hands dirty, but nicotine is also known to quickly and easily pass the skin barrier, which poses a safety concern. In addition, children can accidentally ingest e-liquid and suffer from oral nicotine poisoning.
[0004] Devices for heating tobacco without burning it are an alternative to the E-cigarette. WO 2016 / 026810 and WO 2016 / 207407 describe such heating devices. Tobacco sticks are placed in these heating devices, the tobacco is then heated by the heating device without being burned, which leads to the formation of an aerosol when the user draws air through the device. The generated aerosol has advantageous organoleptic properties when inhaled by the user.
[0005] It may be advantageous to offer the user of these heating devices flavors other than those of tobacco or a neutral flavor. This is why reconstituted plant leaves, such as those described in WO 2019 / 043119, have been developed. Aerosols generated from these reconstituted plant leaves have satisfactory organoleptic properties. However, these reconstituted plant leaves are devoid of nicotine. Consequently, the aerosols generated from these reconstituted plant leaves do not offer a fully satisfactory experience to users of heating devices. heating and smokers since they do not contain nicotine. In addition, these reconstituted plant leaves can be difficult to produce because plant fibers can be difficult to process.
[0006] To solve this technical problem, the inventors tried to add nicotine in neutral form and plant extract to paper sheets. However, they noticed that the nicotine added to the paper sheets can be released during the manufacturing and especially during the storage of the paper sheets and the heating appliance consumables comprising these paper sheets. The aerosols generated from these paper sheets contain nicotine in neutral form, but are not satisfactory because their nicotine quantity is too low and the physiological effect of the neutral form of nicotine on the consumer is too slow. In addition, the aerosols can also be too aggressive.
[0007] To solve this second technical problem, the inventors attempted to stabilize the nicotine by adding an acid to form a nicotine salt. However, they noticed that the aerosols generated from the paper sheets comprising a nicotine salt may still be unsatisfactory because, under certain circumstances: - they contain a quantity of nicotine even lower than that intended, - they are still too aggressive, and / or - they have an unpleasant acidic taste. Technical problem
[0008] There is therefore a need for a nicotine-containing paper sheet that generates an aerosol that is satisfactory to the user.
[0009] It is therefore to the credit of the inventors to have found that it is possible to meet this need by means of a sheet of paper comprising a nicotine salt and having a specific pH range. Summary
[0010] A sheet of paper is provided comprising: - a fibrous support comprising cellulose-based plant fibers, - an aerosol-generating agent, - a plant extract, and - nicotine, a nicotine salt or mixtures thereof, characterized in that the total dry matter content by weight of the cellulose-based plant fibers included in the paper sheet is 22% to 93%, in particular 35% to 85%, more particularly 40% to 83%, and in that. the paper sheet has a pH of 4.9 to 7.0, especially 5.0 to 6.0.
[0011] Advantageously, in these pH ranges, the paper sheet of the present The invention generates an aerosol that delivers nicotine satisfactorily and does not have an unpleasant harshness or acid taste, i.e., an aerosol that is satisfactory to the user.
[0012] The structure of nicotine is such that it comprises two nitrogen atoms capable of accepting protons from an acid and, consequently, nicotine can be present in neutral form (unprotonated form), monoprotonated form and / or diprotonated form. Without wishing to be bound by any theory, the inventors are of the opinion that these results can be explained by: - the monoprotonated form of nicotine which is the main form of nicotine in the paper sheet of the present invention having a pH of 4.9 to 7.0, in particular 5.0 to 6.0. The monoprotonated form of nicotine is stable during the manufacture and storage of the paper sheet of the present invention. In addition, the monoprotonated form of nicotine is efficiently released in the aerosol when using the paper sheet of the present invention in a heating device and is known to have a physiological absorption profile comparable to a conventional cigarette, - the increase in the proportion of the neutral form of nicotine in a paper sheet having a pH above 7. The neutral form is volatile and is therefore easily released during the manufacture and especially during the storage of said paper sheet and heating device consumables comprising said paper sheet.Furthermore, the neutral form causes more irritation and has a slower physiological effect than the monoprotonated form.
[0013] Furthermore, the aerosol generated from a sheet of paper with a pH lower than 4.9 has an unpleasant, harsh and pungent taste and may even have deleterious physiological effects in certain cases, due to the increase in the amount of organic acid in said sheet of paper.
[0014] In addition, the amount of aerosol generated by the paper sheet of the present invention is satisfactory due to the aerosol generating agent.
[0015] Furthermore, since the paper sheet of the present invention is a solid, it does not have the disadvantages of the solution contained in an E-cigarette cartridge. In particular, the nicotine from the paper sheet of the present invention cannot spread onto the user's skin so that said nicotine does not pass the skin barrier and therefore does not pose the safety problem posed by the nicotine of an e-cigarette.
[0016] According to another aspect, there is provided a method of manufacturing a sheet of paper as defined above, comprising the following steps: (a) formation of a solution comprising: - the aerosol-generating agent, - nicotine, nicotine salt or their mixtures, and - the plant extract, b) contacting the solution with a base sheet made from cellulose-based plant fibers to obtain a wet sheet of paper, and c) drying the wet sheet of paper to produce the sheet of paper. Description of the embodiments
[0017] A sheet of paper is provided comprising: - a fibrous support comprising cellulose-based plant fibers, - an aerosol-generating agent, - a plant extract, and - nicotine, a nicotine salt or their mixtures, characterized in that. the total dry matter content by weight of the cellulose-based plant fibers included in the paper sheet is 22% to 93%, in particular 35% to 85%, more particularly 40% to 83%, and the paper sheet has a pH of 4.9 to 7.0, especially 5.0 to 6.0.
[0018] The pH of the paper sheet of the present invention is measured as follows: - grinding the paper sheet to obtain particles smaller than 1 mm, - weighing 5.0 + / - 0.1 mg of ground paper sheet and mixing with 100.0 + / - 0.1 g of deionized water, the resistivity of the deionized water being less than 18.2 Megohm / cm, - magnetic stirring of the sample in water for 15 min at a temperature of 20°C, - pH measurement.
[0019] For the purposes of the present application, the term "fibrous support" designates a base sheet consisting of cellulose-based plant fibers, in particular refined cellulose-based plant fibers. The base sheet is generally obtained by a papermaking process.
[0020] For the purposes of the present application, the term "cellulose-based plant fibers" designates fibers obtained by a chemical or mechanical or thermomechanical pulping process, such as wood fibers, hemp fibers, or fibers from annual plants such as flax fibers for example, in particular wood fibers. A mixture of these cellulose-based plant fibers may also be used.
[0021] Cellulose-based plant fibers give the paper sheet mechanical strength properties.
[0022] The wood fibers may be hardwood pulp, bleached hardwood pulp, softwood pulp, bleached softwood pulp, fluff softwood pulp, lyocell fibers (cellulose fibers ground and dissolved in N-methylmorpholine N-oxide monohydrate to obtain fibers with a variable cross-sectional shape) (round, oval, transverse, circular, lamellar) with a calibrated length and mass per unit length, which the skilled person can choose according to his needs), viscose fibers (fibers obtained by dissolving cellulose by means of the modification of its hydroxyl groups by carbon disulfide (CS2) and precipitation in the presence of sulfuric acid (H2SO4) in order to obtain fibers with a cross section of variable shape (round, oval, transverse, circular, lamellar section) with a calibrated length and mass per unit length, which the skilled person can choose according to his needs) or mixtures thereof, in particular bleached softwood pulp, softwood pulp, fluff softwood pulp, lyocell fibers, viscose fibers or mixtures thereof, more particularly softwood pulp, bleached softwood pulp, or mixtures thereof.
[0023] For the purposes of the present application, the term "refined cellulose-based plant fibers" means cellulose-based plant fibers that have undergone a refining step that allows the fibrillation and / or cutting of the cellulose-based plant fibers. The refining step is conventionally carried out in a papermaking process, such as the papermaking process producing reconstituted paper tobacco.
[0024] For the purposes of the present application, the term "aerosol-generating agent" designates a compound which allows the formation of an aerosol when heated.
[0025] The aerosol-generating agent may be a polyol, a non-polyol, or mixtures thereof. Typically, an aerosol-generating agent that is a polyol may be glycerol, propylene glycol, sorbitol, triethylene glycol, or mixtures thereof. An aerosol-generating agent that is a non-polyol may be glyceryl diacetate, glyceryl triacetate, triethyl citrate, isopropyl myristate, or mixtures thereof.
[0026] The aerosol generating agent may preferably be glycerol, propylene glycol or a mixture of glycerol and propylene glycol, with glycerol being preferred.
[0027] Let Sag be the total content by weight of dry matter of the aerosol-generating agent included in the paper sheet of the present invention. SAG may range from 6% to 70%, in particular from 10% to 65%, more particularly from 15% to 42%.
[0028] The volume of aerosol generated by a sheet of paper having a SAG below the above-mentioned ranges is too low to be pleasant. This aerosol also has no taste.
[0029] For the purposes of the present application, "nicotine salt" designates a form of nicotine characterized by the interaction between nicotine in monoprotonated form or in diprotonated form and an organic acid in carboxylate form.
[0030] In the paper sheet of the present invention, the nicotine salt may be formed in-situ or ex-situ by the reaction between nicotine and an organic acid. Those skilled in the art know that this reaction is an equilibrium. Therefore, the nicotine and the organic acid may be present with the nicotine salt formed in-situ or ex-situ.
[0031] Alternatively, the nicotine salt may be purchased as is and added to the paper sheet of the present invention.
[0032] The total content by weight of nicotine dry matter in the paper sheet may be from 0.1% to 8%, in particular from 0.5% to 4%, more particularly from 0.75% to 3%.
[0033] Advantageously, the nicotine-containing paper sheet in such ranges generates an aerosol that allows the user to obtain a nicotine experience similar to the experience provided by the aerosol generated by a conventional tobacco heating device and by the smoke generated by a combusted tobacco product.
[0034] The paper sheet of the present invention may comprise an organic acid. Advantageously, the pH of the paper sheet of 4.9 to 7.0, in particular 5.0 to 6.0 can be obtained by means of this organic acid. Additionally, the monoprotonated form of nicotine present in the paper sheet of the present invention may result from the formation of a nicotine salt by a reaction between nicotine and the organic acid.
[0035] The pH of the paper sheet of the present invention may depend on the pKa of the organic acid.
[0036] Typically, the organic acid may have: a pKa of less than or equal to 5, in particular less than 4, more particularly less than 3, and a vapor pressure at 25°C of 10 10 to 20 mmHg, in particular of 108 to 10 mmHg, more particularly of 108 to 1 mmHg, a boiling point of greater than or equal to 300°C or both.
[0037] Advantageously, the organic acid having such a pKa and such a vapor pressure and / or such a boiling point: - promotes the formation of nicotine salt in the paper sheet of the present invention with a small amount of organic acid, - limits the transfer of organic acid in the aerosol generated by the paper sheet of the present invention, thus limiting the acid taste of said aerosol, and - limits the loss of acid during the manufacture of the paper sheet of the present invention.
[0038] The organic acid may have several pKas. For example, a dicarboxylic acid has 2 pKas. In this case, the lowest pKa of this organic acid may be less than or equal to 5, in particular less than 4, more particularly less than 3.
[0039] The organic acid may be alginic acid, aspartic acid, benzoic acid, citric acid, fumaric acid, glutamic acid, glycolic acid, lactic acid, levulinic acid, malic acid, pectic acid, pyruvic acid, salicylic acid, tartaric acid, glucuronic acid, galacturonic acid, myristic acid or mixtures thereof, in particular benzoic acid, citric acid, fumaric acid, glycolic acid, lactic acid, levulinic acid, malic acid, pyruvic acid, salicylic acid or mixtures thereof, more particularly benzoic acid, citric acid, malic acid, lactic acid, levulinic acid, salicylic acid or mixtures thereof.
[0040] Advantageously, the organic acids in this list are for the most part products of natural origin, which improves the naturalness of the sheet of paper of the present invention.
[0041] The nicotine:organic acid molar ratio may be from 1:0.1 to 1:10, in particular from 1:0.4 to 1:5, more particularly from 1:0.5 to 1:3. Advantageously, the paper sheet comprising the molar ratio in these ranges may have a pH in the ranges mentioned above.
[0042] For the purposes of the present application, the term "plant extract" designates all the solvent-soluble compounds of the plant. Advantageously, the plant extract comprises compounds conferring organoleptic properties and / or well-being properties to the aerosol. If the plant is a medicinal plant, then the plant extract confers therapeutic properties to the aerosol.
[0043] Typically, the solvent may be an apolar solvent, an aprotic polar solvent, a protic polar solvent or mixtures thereof, in particular the solvent may be methanol, dichloromethane, ethanol, acetone, butanol, supercritical CO2, water or mixtures thereof, more particularly the solvent is ethanol, acetone, water or mixtures thereof, more particularly, the solvent is water.
[0044] An aerosol is generated upon heating the paper sheet of the invention. Advantageously, the plant extract which comprises aromatic compounds imparts aromas of the plant to this aerosol.
[0045] Furthermore, the organoleptic properties can be easily modified by simply changing the plant extract added to the paper sheet.
[0046] The organic acid of the paper sheet may be a compound of the plant extract added to the paper sheet.
[0047] Indeed, the inventors have noticed that a plant extract can give the paper sheet of the present invention a pH of 4.9 to 7.0, in particular 5.0 to 6.0 thanks to the organic acid present in said plant extract. Thus, said plant extract increases the natural character of the paper sheet of the present invention.
[0048] In the case where the plant extract does not give the paper sheet a pH of 4.9 to 7.0, in particular 5.0 to 6.0, the organic acid is then added to the paper sheet to give said paper sheet a pH of 4.9 to 7.0, in particular 5.0 to 6.0. This is particularly true if no organic acid or an insufficient content of organic acid is present in the plant extract.
[0049] Without wishing to be bound by any theory, to determine whether the plant extract gives the paper sheet of the present invention a pH of 4.9 to 7.0, in particular from 5.0 to 6.0, the person skilled in the art can typically measure the pH of the paper sheet comprising a plant extract and devoid of an added organic acid. In one embodiment, the pH of said paper sheet is from 4.9 to 7.0, in particular from 5.0 to 6.0 without added organic acid, the plant extract imparting the correct pH ranges to the paper sheet of the present invention. In another embodiment, the pH of said paper sheet is not 4.9 to 7.0, in particular 5.0 to 6.0, an organic acid must be added during the production process of the paper sheet of the present invention.
[0050] Coffee, ginkgo biloba, star anise, licorice, angelica, sweet flag, caper bush, turmeric, Chinese mahogany, rosehip, tsao-ko or mixtures thereof, in particular coffee, ginkgo biloba, star anise, licorice or mixtures thereof, more particularly ginkgo biloba, star anise or mixtures thereof are an example of a plant whose extract can give the paper sheet of the present invention a pH of 4.9 to 7.0, in particular 5.0 to 6.0 without adding organic acid to said paper sheet.
[0051] The organoleptic properties and the therapeutic properties of the aerosol formed by heating said sheet of paper may depend on the total content by weight of dry matter of the plant extract included in said sheet of paper.
[0052] The total content by weight of dry matter of the plant extract depends on the plant used and, more particularly, on the content of aromatic compounds or compounds having therapeutic or well-being properties of the plant used.
[0053] Let Sp be the total content by weight of dry matter of the plant extract included in the paper sheet of the present invention. Sp may range from 1% to 60%, in particular from 5% to 50%, more particularly from 10% to 35%.
[0054] Advantageously, an Sp included in these ranges of values makes it possible to generate, at a comfortable pull resistance, an aerosol having satisfactory organoleptic properties, that is to say having a constant and high taste intensity and a constant and larger volume.
[0055] To determine SP, the following method can be used: The paper sheet to be analyzed is ground to obtain a particle size less than or equal to 1 mm. The paper sheet is then mixed with boiling water for 45 minutes to extract all of the plant extract. SP is calculated by the difference between the dry weight of the sample of the paper sheet to be analyzed and the dry weight of the fibrous residue after extraction.
[0056] The fibers of the fibrous support may consist of cellulose-based plant fibers.
[0057] Alternatively, the fibrous support may further comprise plant fibers.
[0058] Plant fibers can, for example, come from the same plant or from several plants.
[0059] Typically, the total dry matter weight content of the plant fibers included in the paper sheet may be less than 71%, in particular from 3% to 60%, more particularly from 5% to 55% by dry matter weight of the paper sheet, the remaining fibers of the paper sheet being the cellulose-based plant fibers.
[0060] The plant extract and the plant fibers may be independently obtained from a plant selected from spore-producing plants, seed-producing plants, and mixtures thereof. In particular, the plant may be a plant selected from food plants, aromatic plants, perfume plants, medicinal plants, plants of the Cannabaceae family, and mixtures thereof.
[0061] If the plant is a medicinal plant, the aerosol generated by heating the paper sheet may also have therapeutic properties, so that the paper sheet can be used for therapeutic treatment.
[0062] Advantageously, a plant extract obtained from a mixture of plants makes it possible to offer a wide range of organoleptic properties and / or therapeutic properties. A mixture of plants also makes it possible to counterbalance the unpleasant organoleptic properties of one plant in the mixture, for example a medicinal plant, with the pleasant organoleptic properties of another plant in the mixture, for example an aromatic plant or a perfume plant.
[0063] The plant fibers may be obtained from a first plant and the plant extract may be obtained from a second plant. Indeed, the fibers of a plant may not have mechanical properties allowing the formation of a fibrous support, but the extract of this plant may confer on the aerosol desired organoleptic properties and / or therapeutic properties. Conversely, the fibers of a plant may have mechanical properties allowing the formation of a fibrous support, but the extract of this plant may not confer on the aerosol desired organoleptic properties and / or therapeutic properties.
[0064] Advantageously, the mixture of plants to obtain the plant fibers makes it possible to adjust the mechanical properties of the sheet of paper and / or the organoleptic or chemical properties of the aerosol.
[0065] Typically, food plants are garlic, cardamom, coffee, ginger, lemon verbena, licorice, papaya, stevia, tea, cocoa, chamomile, mate, rooibos, anise such as star anise (or badiane) and green anise, or mixtures thereof, fennel, lemongrass, angelica, caper, turmeric, Chinese mahogany and tsao-ko.
[0066] Aromatic plants are generally basil, turmeric, cloves, bay leaf, oregano, mint, rosemary, sage and thyme.
[0067] Typically, fragrant plants are lavender, marigolds, rose, eucalyptus, sweet flag.
[0068] Typically, medicinal plants are those indicated in the document, list A of medicinal plants traditionally used (French pharmacopoeia January 2016, published by the National Agency for the Safety of Medicines (ANSM) or plants known to include compounds with therapeutic properties. Typically, the medicinal plants listed are ginkgo biloba, ginseng, sour cherry, peppermint, sweet mint, willow and red vine.
[0069] Eucalyptus is one of the medicinal plants known to contain compounds with therapeutic properties.
[0070] Typically, the plant fibers and plant extract of the paper sheet of the present invention may be derived from various parts of the plant, the plant parts being parts of the plant itself or the result of processing various parts of the plant. Typically, the plant parts may be whole parts of the plant or debris from threshing or mixing and shredding the plant parts. The plant parts may also be by-products of extraction.
[0071] Typically, the parts of the plant may be chosen from the parts of the plant richest in aromatic compounds giving the aerosol its organoleptic properties. Typically, these parts may be the whole plant, the aerial parts of the plant, such as the flower bud, the branch bark, the stem bark, the leaves, the flower, the fruit and its peduncle, the seed, the petal, the flowering top, or the underground parts, for example the bulb, the roots, the root bark, the rhizome, or mixtures thereof. The part of the plant may also be the result of the mechanical, chemical or mechanochemical treatment of one or more of the plant, such as for example the shell protecting the cocoa bean resulting from the process of hulling the bean.
[0072] Among the food plants, angelica fruit, angelica bud, angelica root, caper bud, turmeric root, turmeric stem, Chinese mahogany bud, tsao-ko fruit, garlic bulb, coffee cherry, star anise fruit, ginger rhizome, licorice root, rooibos needle, leaf and stem, and stevia, papaya or tea leaves may, for example, be selected as parts.
[0073] Among the aromatic plants, clove flower buds (cloves), basil, bay and sage leaves, leaves and flowering tops of mint, oregano, rosemary and thyme, or even turmeric rhizome can be chosen as a part.
[0074] Typically, among the perfume plants, one can choose the flower and flowering top of lavender, the rhizome of sweet flag, the rosehip or the bud and the petals of the rose flower.
[0075] Among the medicinal plants listed in the French pharmacopoeia, one can for example choose the ginkgo leaf, the underground part of ginseng, the stalk of the morello cherry, the leaves and flowering top of peppermint, the bark of the stem and the leaves of the willow, or even the leaves of the red vine.
[0076] The plant may be tobacco, eucalyptus, angelica, anise such as star anise, green anise or mixtures thereof, hemp, cardamom, cocoa, cannabis, hops, dill, raspberry, bay leaf, nettle, pine, tendu, grape, fennel, lemongrass, lemon verbena, peppermint, spearmint, rooibos, chamomile, flax, ginger, ginkgo biloba, hazelnut, hibiscus, bay leaf, licorice, matcha, star anise, yerba mate, mate, orange peel, papaya, rose, sage, green or black tea, thyme, clove, cinnamon, coffee, basil, bay leaf, cardamom, coriander, cumin, nutmeg, oregano, paprika, rosemary, saffron, lavender, lemon peel, mint, juniper, elderflower, vanilla, wintergreen, perilla, sorrel, turmeric, sandalwood, coriander, bergamot, orange blossom, myrtle, blackcurrant,valerian, chili, mace, damiana, marjoram, olive, lemon balm, lemon basil, chives, caraway, verbena, tarragon, geranium, mulberry, ginseng, theanine, theacrine, maca, ashwagandha, damiana, guarana, chlorophyll, baobab, stevia or mixtures thereof, in particular anise such as star anise, green anise or mixtures thereof, star anise, yerba mate, cocoa, lemon balm, myrtle, lavender, hazelnut, cardamom, cinnamon, eucalyptus, fennel, ginger, ginkgo biloba, mint, peppermint, bay leaf, lemon verbena, liquorice, marigolds, papaya, rooibos, rosemary, sage, sorrel, stevia, tea such as green tea or black tea or mixtures thereof, especially star anise, yerba mate, ginkgo biloba, mint, bay leaf, eucalyptus, cocoa, lemon balm, lemon verbena, myrtle, lavender, hazelnut, green anise, sage,rooibos, tea such as green tea or black tea or their mixtures, more particularly mint or rooibos.
[0077] The plant can be rooibos.
[0078] For example, the plant may be star anise, yerba mate, ginkgo biloba, mint, bay leaf, eucalyptus, cocoa, lemon balm, lemon verbena, myrtle, lavender, hazelnut, green anise, sage, rooibos, tea such as green tea or black tea or mixtures thereof and the organic acid may be benzoic acid, levulinic acid, salicylic acid, lactic acid, malic acid, citric acid or mixtures thereof, in particular salicylic acid, malic acid or mixtures thereof.
[0079] For example, the plant may be star anise, yerba mate, ginkgo biloba, mint, bay leaf, eucalyptus, cocoa, lemon balm, lemon verbena, myrtle, lavender, hazelnut, green anise, sage, rooibos, tea such as green tea or black tea or mixtures thereof and the pH of the paper sheet of the present invention may be 4.9 to 6.0.
[0080] For example, the plant may be star anise, yerba mate, ginkgo biloba, mint, bay leaf, eucalyptus, cocoa, lemon balm, lemon verbena, myrtle, lavender, hazelnut, green anise, sage, rooibos, tea such as green tea or black tea or mixtures thereof, the pH of the paper sheet of the present invention may be 4.9 to 6.0, and the organic acid may be benzoic acid, levulinic acid, salicylic acid, lactic acid, malic acid, citric acid or mixtures thereof, in particular salicylic acid, malic acid or mixtures thereof, more particularly salicylic acid.
[0081] For example, the plant may be mint, particularly spearmint, and the organic acid may be benzoic acid, levulinic acid, salicylic acid, lactic acid, malic acid, citric acid or mixtures thereof, particularly salicylic acid, malic acid or mixtures thereof, more particularly salicylic acid.
[0082] For example, the plant may be mint, particularly spearmint, and the pH of the paper sheet of the present invention may be 4.9 to 7.0, particularly 5.0 to 6.0.
[0083] For example, the plant may be mint, especially spearmint, the pH of the paper sheet of the present invention may be 4.9 to 7.0, especially 5.0 to 6.0, and the organic acid may be benzoic acid, levulinic acid, salicylic acid, lactic acid, malic acid, citric acid or mixtures thereof, especially salicylic acid, malic acid or mixtures thereof, more especially salicylic acid.
[0084] For example, the plant may be rooibos and the organic acid may be benzoic acid, levulinic acid, salicylic acid, lactic acid, malic acid, citric acid or mixtures thereof, in particular salicylic acid, malic acid or mixtures thereof, more particularly salicylic acid.
[0085] For example, the plant may be rooibos and the pH of the paper sheet of the present invention may be 4.9 to 7.0, particularly 4.9 to 6.0.
[0086] For example, the plant may be rooibos, the pH of the paper sheet of the present invention may be 4.9 to 7.0, particularly 4.9 to 6.0, and the organic acid may be benzoic acid, levulinic acid, salicylic acid, lactic acid, malic acid, citric acid or mixtures thereof, particularly salicylic acid, malic acid or mixtures thereof, more particularly salicylic acid.
[0087] Typically, the sheet of paper may have a grammage of less than 300 g / m2, in particular from 15 g / m2 to 200 g / m2, more particularly from 30 g / m2 to 150 g / m2.
[0088] To determine the grammage of the sheet of paper, the following method can be used: A 0.25 m2 sample is cut using a template (dimensions: 57.5 x 43.5 cm) approximately 15 cm from the edge of the sheet of paper to be analyzed. The sample is then folded in four and placed on a hot plate to be dried to remove the water without removing the aerosol-generating agent. The dried sample is then weighed to determine the basis weight of the sheet of paper.
[0089] According to another embodiment, the sheet of paper may comprise: - a fibrous support comprising cellulose-based plant fibers, in particular consisting of cellulose-based plant fibers, - an aerosol-generating agent, - a plant extract, and - nicotine, a nicotine salt or mixtures thereof, characterized in that the total dry matter content by weight of the cellulose-based plant fibers included in the paper sheet is 30% to 90%, in particular 45% to 65%, the paper sheet comprises an organic acid, especially salicylic acid, the plant of the plant extract is mint, especially sweet mint, and the paper sheet has a pH of 4.9 to 7.0, especially 5.0 to 5.5.
[0090] Also provided is a method of manufacturing a sheet of paper as defined above, comprising the following steps: (a) formation of a solution comprising: - the aerosol-generating agent, - nicotine, nicotine salt or their mixtures, and - plant extract , b) contacting the solution with a base sheet made from cellulose-based plant fibers to obtain a wet sheet of paper, and (c) drying the wet paper sheet to produce the paper sheet.
[0091] The cellulose-based plant fibers, the aerosol-generating agent, the plant extract, the nicotine and the nicotine salt are as defined above in relation to the paper sheet of the present invention.
[0092] The base sheet may be produced by passing the cellulose-based plant fibers through a paper machine. Therefore, the paper sheet of the invention may be a paper sheet obtained by a papermaking process.
[0093] The solution formed in step a) and used in step b) may comprise an organic acid as defined above in relation to the sheet of paper of the present invention.
[0094] In the solution formed in step a) and used in step b), the nicotine:organic acid molar ratio may be from 1:0.1 to 1:10, in particular from 1:0.4 to 1:5, more especially 1:0.5 to 1:3.
[0095] The pH of the solution formed during step a) and used in step b) may be acidic, in particular from 3.5 to 6.0, more particularly from 4.3 to 5.2. Advantageously, a solution having a pH in these ranges can enable the production of the paper sheet of the present invention.
[0096] The pH of the solution depends mainly on the amount of organic acid, nicotine and / or nicotine salt in said solution. The person skilled in the art knows how to adjust the amount of organic acid, nicotine and / or nicotine salt in the solution so that the latter has a pH within the range mentioned above.
[0097] The inventors have noted that the pH and buffering capacity of the base sheet may depend on the type of fibers. The pH of the solution may therefore be adapted to the pH and buffering capacity of the base sheet to enable the production of the paper sheet of the present invention.
[0098] The pH of the solution is determined using a pH electrode. The pH of the base sheet is determined by the method described above for determining the pH of the paper sheet of the present invention.
[0099] The paper sheet produced by the process of the present invention, and therefore the base sheet of step b), may further comprise plant fibers. The plant fibers are as defined above in relation to the paper sheet of the present invention. Accordingly, a mixture of cellulose-based plant fibers and plant fibers can be passed through a paper machine to produce the base sheet used in step b).
[0100] The plant fibers and the plant extract can be obtained according to the following steps: (d) mixing one or more parts of the plant with a solvent in order to extract the plant extract from the plant fibers, and e) separation of the plant extract from the plant fibers.
[0101] The plant extract and the plant fibers are thus typically obtained by means of a dissociation process. In step d), one or more plant parts are mixed with a solvent, for example in a digester, in order to extract the plant extract from the plant fibers. In step e), the plant extract is separated from the plant fibers, for example by passing through a screw press, in order to isolate and obtain, on the one hand, the plant fibers and, on the other hand, the plant extract.
[0102] Typically, the solvent may be an apolar solvent, an aprotic polar solvent, a protic polar solvent, or mixtures thereof, in particular the solvent may be methanol, dichloromethane, ethanol, acetone, butanol, CO2 super critical, water or their mixtures, more particularly the solvent is ethanol, acetone, water or their mixtures.
[0103] The solvent may be an aqueous solvent, more particularly water.
[0104] The person skilled in the art knows how to adjust the temperature of the solvent during step d) to the plant, the plant part and the plant parts to be treated. Typically, the solvent temperature during treatment of a root or bark will be higher than the solvent temperature during treatment of a leaf or petal.
[0105] Typically, the temperature of the solvent during step d) may be from 10°C to 100°C, in particular from 30°C to 90°C, more particularly from 40°C to 80°C.
[0106] Typically, plant fibers may be refined in a refiner to produce the base sheet.
[0107] Typically, plant fibers can come from different plants.
[0108] The fibers of each plant can be obtained separately according to the dissociation process described above. They can then be mixed so that this mixture of fibers from various plants passes through the paper machine so as to constitute the fibrous support. It is also possible to obtain fibers from various plants together by bringing together one or more parts of the various plants and then subjecting them to the dissociation process described above. The water temperature will then be adapted to the plants to be treated and, in particular, to the plant requiring the highest water temperature for the extraction of the extract from this plant. This variant embodiment is very advantageous because it makes it possible to obtain the fibers from the different plants without carrying out several dissociation processes in parallel.
[0109] Typically, the plant extract may be an extract of various plants.
[0110] The extract of various plants can be obtained by mixing various plant extracts obtained separately according to the dissociation process described above. It is also possible to obtain the extract of various plants by combining one or more parts of the various plants and then subjecting them to the dissociation process described above. The water temperature will then be adapted to the plants to be treated and in particular to the plant requiring the highest water temperature for the extraction of the water-soluble extract from this plant. This variant embodiment is very advantageous because it makes it possible to obtain the extract of different plants without carrying out several processes in parallel. In these two situations, the extracts of various plants are used in step a).
[0111] The solution may be formed during step a) by mixing in a solvent, in particular water, the nicotine, the aerosol-generating agent, the organic acid and optionally the plant extract. As a result, the nicotine salt is formed in situ in the solution by reaction between the organic acid and the nicotine. In particular, during this step a): - the organic acid can be mixed with nicotine to form a mixture. Indeed, it advantageously promotes the formation of nicotine salt, - the aerosol-generating agent and possibly the plant extract can then be added to this mixture to form a second mixture, - the solvent, in particular water, is then added to this second mixture to form the solution. The solution can be heated, if necessary, from 40°C to 60°C. This heating step promotes the solubilization of the components in the solution.
[0112] Typically, the plant extract may be concentrated before being added to the solution during step a). A device such as a vacuum evaporation device may be used to concentrate the plant extract.
[0113] Typically, step b) can be carried out by impregnation or by spraying, in particular by impregnation. Typically, the impregnation can be carried out by means of a size press.
[0114] Typically, the drying step c) can be carried out by infrared ramp, American battery drying rollers, hot air drying in a tunnel dryer, a vertical dryer, a fluidized bed dryer, a pneumatic dryer, in particular in a tunnel dryer.
[0115] The sheet of paper produced in step c) can be shaped into particles, into creped sheet form, or into shredded form.
[0116] The paper sheet of the invention can be used in an aerosol generating system.
[0117] Thus, there is also provided a consumable for an aerosol generation system comprising a sheet of paper according to the invention as defined above.
[0118] For the purposes of the present invention, the term "consumable" designates the sheet of paper according to the invention as such, a sachet comprising the sheet of paper according to the invention, a capsule comprising the sheet of paper according to the invention or a stick for a heating device comprising the sheet of paper according to the invention.
[0119] For the purposes of the present application, the expression "aerosol generating system" means any device allowing the formation of an aerosol intended to be inhaled by a consumer. The aerosol provides nicotine to the consumer. Furthermore, thanks to the aerosol generating system, the formation of harmful components during combustion is avoided, which very significantly reduces the exposure of the consumer to said harmful components.
[0120] Typically, an aerosol generation system comprises, in the direction of the air flow, an air inlet, a heating body, a housing intended to place and maintain the consumable of the invention, and an air outlet intended to be introduced into the user's mouth. The air inlet, the heating body, the housing and the air outlet are typically at least fluidly connected to each other.
[0121] When using the aerosol generating system, air is drawn into the aerosol generating system via the air inlet by the user; the drawn air then passes into the heated portion so as to obtain heated air; upon contact with the sheet of paper of the invention comprising the aerosol generating agent, held in the housing, an aerosol is formed and is then inhaled by the user.
[0122] The aerosol generating system may be a tobacco heating-without-burning device (such as IQOS™ or glo™), an E-cigarette (such as Vuse), an herbal vaporizer (such as Pax®), or a hybrid technology (such as Ploom™ Tech).
[0123] The consumable is adapted to be introduced into a dedicated housing of the aerosol generating system, and those skilled in the art will know how to adapt the consumable according to the dedicated housing of the aerosol generating system.
[0124] The paper sheet according to the invention, as a consumable, can be shaped so as to fit the dedicated housing of the aerosol generation system. For example, it can be in the form of particles, in the form of a creped sheet, in the form of a shredded sheet, in particular in the form of a shredded sheet having a width of 0.5 mm to 1 mm.
[0125] The bag may be made of paper with an inner volume and the sheet of paper according to the invention is contained in the inner volume. In the inner volume, the sheet of paper according to the invention may be shaped, in particular in the form of particles, creped sheets or shredded sheets.
[0126] The sheet of paper according to the invention may in particular be in the form of a shredded sheet in a stick for an aerosol generation system.
[0127] According to one embodiment, the sheet of paper included in the consumable product can be obtained by the method according to the invention as defined above.
[0128] It is also proposed to use a sheet of paper according to the invention as defined above or a consumable according to the invention as defined above in an aerosol generation system.
[0129] The sheet of paper according to the invention, as defined above, can also be used as packaging paper.
[0130] Also provided is a non-therapeutic use of a consumable product as defined above in an aerosol generating system.
[0131] A consumable as defined above is also provided for use in an aerosol generation system, the plant being chosen from medicinal plants. Examples
[0132] Example 1: Manufacture of sheets of paper.
[0133] Example 1-1: according to the invention
[0134] The following protocol is used to make the two sheets of paper of Example 1-1 shown in Table 1 below.
[0135] Cellulose-based plant fibers are passed through a laboratory paper machine to obtain a base sheet.
[0136] The organic acid is mixed with the nicotine to form a mixture. The glycerol and the plant extract are then added to this mixture to form a second mixture. Water is added to this second mixture. This latter mixture is heated to 48°C and stirred until completely dissolved to form a solution.
[0137] The solution is added to the base sheet by impregnation in a sizing press so as to obtain, after drying, the sheet of paper.
[0138] Example 1-2 not in accordance with the invention
[0139] The following protocol is used to make the two sheets of paper of Example 1-2 shown in Table 1 below.
[0140] Cellulose-based plant fibers are passed through a laboratory paper machine to obtain a base sheet.
[0141] Glycerol and plant extract are mixed with nicotine to form a mixture. Water is added to this mixture. This final mixture is heated to 48°C and stirred until completely dissolved to form a solution.
[0142] The solution is added to the base sheet by impregnation in a sizing press so as to obtain, after drying, the sheet of paper.
[0143] Example 2: Determination of nicotine release.
[0144] Example 2A: high temperature aging.
[0145] The paper sheets of Example 1-1 and Example 1-2 are stored for 11 days under the following conditions: 40°C, 60% relative humidity.
[0146] The total nicotine dry matter weight content of these examples is then measured by gas chromatography coupled with a flame ionization detector (GC-FID). For each sheet of paper, the nicotine loss after storage is shown in Table 1 below.
[0147] The results, presented in Table 1, demonstrate that nicotine is stabilized in the paper sheet according to the present invention having a pH between 4.9 and 7.
[0148] [Tableauxl] Example 1-1 Example 1-2 not in accordance with the invention Cellulose-based plant fibers Unbleached and refined wood pulp Bleached and refined wood pulp Unbleached and refined wood pulp Bleached and refined wood pulp Organic acid Salicylic acid No acid Plant extract Sweet mint Rooibos Sweet mint Rooibos pH of the paper sheet 5.2 4.9 7.5 7.3 Content by weight of dry matter of cellulose-based plant fibers 49.0% (±0.7%) 62.8% (±0.7%) 52.3% (±0.7%) 62.3% (±0.7%) Total content by weight of nicotine dry matter 1.99% (±0.07%) 1.70% (±0.07%) 1.63% (±0.07%) 1.53% (±0.07%) Dry matter content of plant extract 26.3% (±0.9%) 14.2% (±0.9%) 27.4% (±0.9%) 15.8% (±0.9%) Dry matter content of glycerol 20.3% (±0.7%) 19.3% (±0.7%) 18.7% (±0.7%) 20.2% (±0.7%) Nicotine: organic acid molar ratio 1:1.8 1:1.4 / / Grammage (gm )-2 77 63 77 63 pH of solution 4.7 4.5 8.2 7.2 Nicotine loss 1 5 45 35 after storage (%)
Claims
Claims
1. A paper sheet comprising: - a fibrous support comprising cellulose-based plant fibers, - an aerosol-generating agent, - a plant extract, and - nicotine, a nicotine salt or mixtures thereof, characterized in that the total dry matter weight content of the cellulose-based plant fibers included in the paper sheet is 22% to 93%, and the paper sheet has a pH of 4.9 to 7.
0.
2. The paper sheet of claim 1, wherein the paper sheet further comprises an organic acid.
3. A paper sheet according to claim 2, wherein the organic acid is alginic acid, aspartic acid, benzoic acid, citric acid, fumaric acid, glutamic acid, glycolic acid, lactic acid, levulinic acid, malic acid, pectic acid, pyruvic acid, salicylic acid, tartaric acid, glucuronic acid, galacturonic acid, myristic acid or mixtures thereof.
4. A paper sheet according to any one of claims 1 to 3, wherein the total nicotine solids content by weight is 0.1% to 8%.
5. A paper sheet according to any one of claims 1 to 4, wherein the fibrous support further comprises plant fibers.
6. A paper sheet according to claim 5, wherein the total dry matter weight content of the plant fibers included in the paper sheet is less than 71%.
7. A sheet of paper according to any one of claims 1 to 6, wherein the plant is chosen from food plants, aromatic plants, perfume plants, medicinal plants, plants of the Cannabaceae family, and mixtures thereof.
8. A paper sheet according to any one of claims 2 to 7, wherein the organic acid of the paper sheet is a compound of the plant extract added to the paper sheet.
9. A paper sheet according to claim 8, wherein the plant of the plant extract is coffee, ginkgo biloba, star anise, licorice, angelica, sweet flag, caper, turmeric, Chinese mahogany, rosehip, tsao-ko or mixtures thereof.
10. A method of manufacturing a paper sheet as defined in any one of claims 1 to 9, comprising the following steps: a) forming a solution comprising: - the aerosol generating agent, - nicotine, nicotine salt or mixtures thereof, and - the plant extract, b) contacting the solution with a base sheet made from cellulose-based plant fibers to obtain a wet paper sheet, and c) drying the wet paper sheet to produce the paper sheet.
11. The method of claim 10, wherein the solution formed in step a) and used in step b) further comprises an organic acid.
12. A method according to claim 10 or claim 11 for producing a paper sheet as defined in any one of claims 5 to 7, wherein a mixture of cellulose-based plant fibers and plant fibers is passed through a paper machine so as to produce the base sheet used in step b).
13. A consumable for an aerosol generating system comprising a sheet of paper as defined in any one of claims 1 to 9.
14. Non-therapeutic use of a consumable as defined in claim 13 in an aerosol generating system.
15. Consumable for use in an aerosol generating system for therapeutic purposes, wherein the consumable comprises a sheet of paper as defined in any one of claims 1 to 9 and the plant is selected from medicinal plants.
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