EP3232825A1 - An oral smokeless moist snuff product - Google Patents

An oral smokeless moist snuff product

Info

Publication number
EP3232825A1
EP3232825A1 EP15820112.9A EP15820112A EP3232825A1 EP 3232825 A1 EP3232825 A1 EP 3232825A1 EP 15820112 A EP15820112 A EP 15820112A EP 3232825 A1 EP3232825 A1 EP 3232825A1
Authority
EP
European Patent Office
Prior art keywords
weight
oral smokeless
moist snuff
flavorant
smokeless moist
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP15820112.9A
Other languages
German (de)
French (fr)
Other versions
EP3232825B1 (en
Inventor
Henrik SAHLÉN
Mårten KINDVALL
Christian WERDINIUS
Martin Sjögren
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Swedish Match North Europe AB
Original Assignee
Swedish Match North Europe AB
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Swedish Match North Europe AB filed Critical Swedish Match North Europe AB
Priority to SI201530515T priority Critical patent/SI3232825T1/en
Publication of EP3232825A1 publication Critical patent/EP3232825A1/en
Application granted granted Critical
Publication of EP3232825B1 publication Critical patent/EP3232825B1/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B13/00Tobacco for pipes, for cigars, e.g. cigar inserts, or for cigarettes; Chewing tobacco; Snuff
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/28Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/281Treatment of tobacco products or tobacco substitutes by chemical substances the action of the chemical substances being delayed
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/28Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/281Treatment of tobacco products or tobacco substitutes by chemical substances the action of the chemical substances being delayed
    • A24B15/282Treatment of tobacco products or tobacco substitutes by chemical substances the action of the chemical substances being delayed by indirect addition of the chemical substances, e.g. in the wrapper, in the case
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/28Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/281Treatment of tobacco products or tobacco substitutes by chemical substances the action of the chemical substances being delayed
    • A24B15/283Treatment of tobacco products or tobacco substitutes by chemical substances the action of the chemical substances being delayed by encapsulation of the chemical substances
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/28Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/30Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
    • A24B15/302Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
    • A24B15/303Plant extracts other than tobacco
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/28Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/42Treatment of tobacco products or tobacco substitutes by chemical substances by organic and inorganic substances

Definitions

  • the present disclosure relates to oral smokeless moist snuff products containing particles, such as microparticles, for flavor release.
  • the disclosure also relates to methods for making such products and uses thereof.
  • Smokeless tobacco for oral use includes chewing tobacco, dry snuff and moist (wet) snuff.
  • dry snuff has moisture content of less than 10 wt% and moist snuff has a moisture content of above 40 wt%.
  • Semi-dry products having between 10% to 40 wt% moisture content are also available.
  • Smokeless tobacco products for oral use are made from tobacco leaves, such as lamina and stem of the tobacco leaf.
  • the material from roots and stalks are normally not utilized for production of smokeless tobacco compositions for oral use.
  • American-type moist snuff is available in a loose form or as pre-packed pouches and is typically used between the lower gum and lip.
  • the use of American-type moist snuff is commonly called dipping.
  • Snus is the Scandinavian-type of moist snuff which is also available in loose form or as pre-packed portions in pouches. Snus is typically used between the upper gum and lip.
  • American-type moist snuff is commonly produced through a fermentation process of moisturized ground or cut tobacco.
  • Scandinavian-type moist snuff (snus) is commonly produced by using a heat-treatment process (pasteurization) instead of fermentation.
  • the heat-treatment is carried out in order to degrade, destroy or denature at least a portion of the microorganisms within the tobacco preparation.
  • the tobacco preparation subjected to this heat-treatment process normally has moisture content within the range of from about 22 to 44% w/w.
  • additional water, salt, pH adjuster and additional ingredients, such as flavours are added to the tobacco preparation after this heat-treatment in order to provide the final smokeless tobacco composition, such as the moist snuff.
  • the main ingredients of oral smokeless moist snuff are tobacco, water, sodium carbonate, sodium chloride and a humectant such as propylene glycol or glycerol. Often a flavorant is present to enhance the organoleptic experience by a consumer. Instead of tobacco, fibres of non-tobacco plant material may be used thereby providing an oral smokeless non- tobacco product.
  • the organoleptic properties such as texture, aroma, taste, form and package of the product are of high importance for the consumer.
  • a way of changing and/or improving the sensory experience by a consumer is to add a flavorant to the tobacco material.
  • the flavorant may be added by mixing it with the tobacco material.
  • the oral smokeless tobacco product is placed in a consumer ' s oral cavity the natural tobacco flavor and/or the added flavorant will be extracted by the consumer ' s saliva.
  • the flavorant is extracted gradually. After a certain time, such as about one hour, the consumer usually perceives the taste as gone and therefore disposes the product.
  • the flavorant may be added to the tobacco formulation in a form that physically separates it from the tobacco formulation.
  • particles containing a flavorant may be added.
  • the particles containing a flavorant may be provided as a capsule, such as a encapsulated. Disintegration of the capsule leads to flavor release.
  • the capsules may be designed so that flavor release only takes place when certain conditions are fulfilled. For instance, the capsules may be temperature sensitive so that a certain temperature is required for capsule disintegration and concomitant flavor release. Further, encapsulation of the flavorant prevents it from interacting with the tobacco composition and/or the atmosphere in the container for the tobacco composition.
  • the microcapsule shell comprises gelatine. During storage in a refrigerator or at room temperature (i.e. about 22 °C) the gelatine shell maintains its integrity and does not
  • the capsule material must maintain its 10 integrity and substantially withstand leakage of the enclosed flavorant when mixed and stored together with the moist tobacco composition.
  • the capsule material should be able to disintegrate and provide controlled release of the flavorant when the oral smokeless moist snuff product is placed in a user ' s mouth.
  • microencapsulated flavorants A list of outer wall or shell material of the microcapsules is mentioned, said list including inter alia gelatine and hydroxypropyl methylcellulose. It is stated that microencapsulated tobacco flavorants will provide extended release of the tobacco flavor under conditions of normal use of the smokeless tobacco product, such as
  • smokeless tobacco product may lose their physical integrity when the smokeless tobacco product reaches a certain pH or a certain temperature.
  • US 2004/0180067 discloses a particle composition containing a continuous phase of 5- 25 95% organically soluble cellulosic material selected from the group consisting of ethyl cellulose and hydroxypropyl cellulose dissolved in 5-95% organic fragrance chemicals and organic flavor chemicals. It is stated that a particle formed of hydroxypropyl cellulose and flavor will not dissolve in an aqueous solution of 10% NaCI, although flavor chemicals will partition into the aqueous phase over time.
  • WO 2009/073190 discloses a fast-dissolving film for use as a platform for the delivery of material to the oral cavity, comprising a film forming agent, a plasticizing agent and a water-soluble agent.
  • the material may be nicotine.
  • the film may be edible and is fast- dissolving upon contact with water-based aqueous systems such as human saliva.
  • WO2009/056609 discloses oral smokeless tobacco compositions comprising
  • the encapsulating agent is hydrophobic and poorly soluble in aqueous solutions.
  • the release of the flavourant may be caused by alteration/degradation of the encapsulating agent with saliva and/or thermal degradation, e.g. melting of the encapsulation agent at a temperature present in the oral cavity.
  • US 2010/0282267 discloses an encapsulated flavorant for use with smokeless tobacco.
  • the encapsulated flavorant comprises a core with a lipid-based coating that provides stability when in contact with tobacco, yet releases flavor over time when the product is used.
  • an oral smokeless moist snuff product comprising:
  • salts selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combination thereof, and
  • the total amount of the one or more salts is within the range of from about 15 % by weight to about 35 % by weight based on the total weight of water and total weight of the one or more salts in the oral moist smokeless snuff composition, wherein the total amount of moisture is within the range of from about 35 % by weight to about 60 % by weight based on the total weight of the oral smokeless moist snuff composition;
  • particles comprising a flavorant and a cellulose-derivatized polymer selected from the group consisting of hydroxypropyl methylcellulose, hydroxypropyl cellulose, methyl cellulose and any combination thereof,
  • the amount of said particles is within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product.
  • an oral smokeless moist snuff product comprising:
  • an oral smokeless moist snuff composition as described herein (a) an oral smokeless moist snuff composition as described herein, and (b) particles comprising a flavorant and a cellulose-derivatized polymer selected from the group consisting of hydroxypropyl methylcellulose, hydroxypropyl cellulose, methyl cellulose and any combination thereof, said particles being as defined herein.
  • an oral smokeless moist snuff product comprising:
  • salts selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combination thereof, and
  • the total amount of the one or more salts is within the range of from about 15 % by weight to about 35 % by weight based on the total weight of water and total weight of the one or more salts in the oral moist smokeless snuff composition, wherein the total amount of moisture is within the range of from about 35 % by weight to about 60 % by weight based on the total weight of the oral smokeless moist snuff composition; (b) particles comprising a flavorant and a cellulose-derivatized polymer selected from the group consisting of hydroxypropyl methylcellulose, hydroxypropyl cellulose, methyl cellulose and any combination thereof,
  • the amount of said particles is within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the present disclosure is based on the finding that gelatine microcapsules containing a flavorant when in admixture with an oral smokeless moist snuff composition soften and/or disrupt upon storage even in the presence of a quite large amount of salt.
  • oral smokeless moist snuff products are stored in refrigerators or at room temperature making storage stability at temperatures within the range of from about 5 to about 25 °C important.
  • storage stability at slightly lower or higher temperature may be desirable. For instance, storage at about 0°C or about 30-45°C may be important.
  • Common storage times range from two weeks to six months.
  • the flavor profile of the oral smokeless tobacco product described herein, such as the oral smokeless moist snuff product, is such that flavorant release substantially takes place after the oral smokeless tobacco product has been placed into a user ' s mouth.
  • flavorant release substantially takes place after the oral smokeless tobacco product has been placed into a user ' s mouth is such that flavorant release substantially takes place after the oral smokeless tobacco product has been placed into a user ' s mouth.
  • the flavorant release may take place during an extended period of time such as about one hour.
  • the flavor intensity experienced by a user may increase over time so that the experienced flavor intensity is higher at the end of usage than at the beginning.
  • a user may experience the flavor intensity to be substantially constant.
  • storage stability refers to the ability of a product to substantially withstand alteration and/or degradation during storage.
  • the product may be the oral smokeless moist snuff product described herein and/or the particles containing a flavorant described herein.
  • the particles containing a flavorant are considered to be storage stable when they substantially maintain their integrity during storage.
  • storage stability may refer to storage stability at about room temperature, i.e. about 20-25 °C such as about 22 °C, during about three weeks. In a further example, storage stability may refer to storage stability at about 5 °C during about twenty weeks.
  • An oral smokeless moist snuff product may be considered to be storage stable when at least about 75 %, such as about 80%, about 85%, about 90%, about 95% or about 100%, of the total flavor of the flavorant particles remains encapsulated.
  • the total flavour intends the sum of the flavor of the particles containing a flavorant and the flavor contained in the oral smokeless moist snuff composition. The total flavor may be determined as described in the experimental section of this document.
  • the one or more salts selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate and potassium lactate and any combinations thereof act by lowering the cloud point of the cellulose-derivatized polymer enclosing the flavorant.
  • the polymer cloud point defines the temperature above which the cellulose-derivatized polymer is insoluble, and below which it is soluble.
  • the particles such as the microcapsules or granules maintain their integrity at a temperature from about 0 °C to about 50°C, such as from about 5 °C to about 45°C or at body temperature (i.e. about 37°C).
  • concentration of the one or more salts is lowered the particles such as the microcapsules or granules soften and/or disintegrate thereby releasing the encapsulated flavorant. Therefore, when the oral smokeless moist snuff product described herein is placed in a user ' s mouth saliva excretion lowers the salt concentration leading to microcapsule softening and disintegration followed by extended flavorant release. This is in contrast to, for example, thermosensitive microcapsules in which a mere temperature change results in capsule disintegration.
  • the salting out of polymers leading to polymer cloud point lowering is known in other technical fields.
  • the tobacco or the non- tobacco plant fibres contain a large number of components which may influence the polymer cloud point.
  • other components that are frequently present in oral smokeless moist snuff may also have an impact on the cellulose-derivatized polymer cloud point. It is therefore a complex task to provide an oral smokeless moist snuff product wherein extended flavor release substantially takes place after having placed the product into a user ' s mouth.
  • the disintegrated plant material may be disintegrated tobacco or disintegrated non- tobacco plant fibres as described herein.
  • disintegrate(d) is understood to mean cut, ground and/or shredded.
  • the disintegrated plant material may be shredded.
  • the disintegrated plant material may be finely disintegrated, i.e. it has an average particle size of less than 2 mm.
  • the particles of the finely disintegrated plant material, such as finely disintegrated tobacco material may be sized to pass through a screen of about 10 (US) mesh, i.e. sieve size 2.0 mm, or 18 (US) mesh, i.e. sieve size 1 .0 mm.
  • the term "snuff' used in the context of oral smokeless moist snuff composition and/or oral smokeless moist snuff product may intend fermented snuff and/or pasteurized snuff.
  • the snuff may be American-type moist snuff and/or
  • An oral smokeless moist tobacco composition is an oral smokeless moist snuff composition wherein the disintegrated plant material comprises or consists of tobacco. Addition of particles containing a flavorant as described herein to the oral smokeless moist tobacco composition provides an oral smokeless moist tobacco product.
  • the tobacco may be mixed with non-tobacco fibres as decribed herein.
  • An oral smokeless moist non-tobacco composition is an oral smokeless moist snuff composition wherein the disintegrated plant material comprises or consists of non-tobacco fibres. Addition of particles containing a flavorant as described herein to the oral smokeless moist non-tobacco composition provides an oral smokeless non-tobacco product.
  • the oral smokeless moist non-tobacco composition and/or the oral smokeless non-tobacco product does not comprise tobacco material such as disintegrated tobacco.
  • the tobacco may be any part, e.g. leaves or stems, of any member of the genus
  • the tobacco may be whole or disintegrated, i.e. shredded, cut, ground, cured. Further, the tobacco may be aged, fermented or treated otherwise.
  • the tobacco may include types of material such as flue-cured tobacco, burley tobacco, oriental tobacco, Maryland tobacco, dark tobacco, dark-fired tobacco, dark air cured or light air cured and Rustica tobaccos as well as other rare or specialty tobaccos.
  • the tobacco of the present disclosure may contain a single type of tobacco or different types of tobacco.
  • the tobacco can have the form of processed tobacco parts or pieces, cured and aged tobacco in substantially natural lamina or stem form, a tobacco extract, extracted tobacco pulp or a mixture of the foregoing.
  • the tobacco may be mixed together with non-tobacco fibres.
  • the tobacco contains salt such as sodium chloride and/or potassium chloride.
  • the total chloride content i.e. the chloride originating from chloride salts such as sodium and potassium chloride, may be within the range of from about 3 to about 8 % by weight such as from about 3 to about 6 % by weight based on the weight of the tobacco flour, said tobacco flour may contain about 7 % by weight of water.
  • the chloride content of the disintegrated tobacco or the disintegrated non-tobacco plant material may be about 3 % by weight or about 4 % by weight based on the weight of the tobacco flour, said tobacco flour may contain about 7 % by weight of water.
  • the non-tobacco plant fibres may be fibres from non-tobacco plants such as maize fibers, oat fibers, tomato fibers, barley fibers, rye fibers, sugar beet fibers, buck wheat fibers, potato fibers, cellulose fibers, apple fibers, cocoa fibers, bamboo fibers and citrus fibers.
  • the non-tobacco plant fibres may be whole or disintegrated, i.e. shredded, cut, ground. Further, the non-tobacco plant fibres may be cured, aged, fermented or treated otherwise.
  • the amount of non-tobacco plant fibers, such as bamboo fibers, in the smokeless tobacco composition may be within the range of from about 1 to about 60% w/w or from about 2 to about 20% w/w based on dry weight of the smokeless tobacco composition.
  • Micro Crystalline Cellulose may also be used as an alternative.
  • the non-tobacco fibers may have an average length-to-width ratio equal to or greater than 3.5:1 and equal to or lower than 100:1 .
  • the non-tobacco plant fibers may originate from bamboo.
  • the non-tobacco fibers may have an average length-to-width ratio equal to or lower than 25:1 .
  • the non-tobacco fibers may have an average length-to-width ratio equal to or greater than 6:1.
  • the non-tobacco fibers may have an average length-to-width ratio equal to or greater than 10:1 .
  • the non-tobacco fibers may have an average length- to- width ratio equal to or greater than 15:1.
  • the oral smokeless moist snuff product described herein may be provided in particulate form, as a loose powder, or be portion-packaged in a pouch.
  • the pouch may be made of a water-permeable material so that extraction of components such as nicotine and/or flavorant may easily take place when the product is placed in a user ' s mouth.
  • the encapsulation of the flavorant in the microcapsule or granule may be encapsulation of the flavorant by a shell such as a coating.
  • the flavorant encapsulation may be that the flavorant is contained in a matrix.
  • the flavorant may be dispersed within a matrix.
  • the matrix may be enclosed by a shell or coating.
  • the shell and/or the matrix may comprise or consist of a cellulose-derivatized polymer selected from the group consisting of hydroxypropyl methylcellulose,
  • an oral smokeless moist snuff product as described herein wherein the flavorant is encapsulated by a coating comprising a cellulose-derivatized polymer as described herein.
  • the cellulose-derivatized polymer may be hydroxypropyl
  • the cellulose-derivatized polymer described herein may be mixed with further ingredients.
  • the cellulose-derivatized polymer may be mixed with talcum powder.
  • hydroxypropylmethyl cellulose may be mixed with talcum powder.
  • the microcapsule or granule flavorant of the oral smokeless moist snuff product described herein is encapsulated by an inner coating and an outer coating.
  • the inner coating may comprise or consist of gelatine.
  • the outer coating may comprise or consist of a cellulose-derivatized polymer selected from the group consisting of hydroxypropyl methylcellulose, hydroxypropyl cellulose, methyl cellulose and any combinations thereof.
  • the outer coating may comprise or consist of hydroxypropyl methylcellulose.
  • the inner coating comprises or consists of gelatine
  • the outer coating comprises or consists of hydroxypropyl methylcellulose optionally in combination with talcum powder.
  • the outer coating is salt-sensitive so that it substantially remains in a solid state in the presence of a salt selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate and potassium lactate and any combinations thereof in the amounts indicated herein.
  • the salt concentration is lowered, such as upon saliva excretion in a user ' s mouth, the outer coating softens and/or dissolves so that the gelatine inner coating is exposed.
  • the outer coating should cover most of the inner coating.
  • the outer coating should be free or substantially free from cracks.
  • the oral smokeless moist snuff product described herein comprises one or more salts selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combinations thereof.
  • the sodium chloride may be replaced entirely or partly with potassium chloride.
  • the one or more salts when the one or more salts is a combination of different salts each salts may be present in an amount sufficient to contribute to cellulose-derivatized polymer cloud point lowering in the oral smokeless moist snuff product.
  • the one or more salts of the oral smokeless moist snuff product described herein may comprise or consist of sodium chloride, sodium carbonate and potassium sulphate.
  • the one or more salts of the oral smokeless moist snuff product described herein may comprise or consist of sodium sulphate and/or potassium sulphate and one or more salts selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate and any combination thereof.
  • the one or more salts of the oral smokeless moist snuff product described herein comprises sodium carbonate, sodium chloride and optionally one or more salts selected from the group consisting of potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combination thereof.
  • the sodium chloride may be replaced entirely or partly with sodium sulphate or potassium sulphate. Replacing the sodium chloride with sodium sulphate and/or potassium sulphate may affect the flavour profile of the product, which may be desirable to meet the demands of certain users.
  • sodium chloride may be exchanged for sodium sulphate and/or potassium sulphate to at least some extent without affecting the cloud point of the cellulose-derivatized polymer of the particles containing a flavorant.
  • the one or more salts may be mixed with the disintegrated plant material such as tobacco or with the non-tobacco plant fibres. Additionally, the one or more salts may be contained in the microcapsules. As an example, the one or more salts may be contained in the microcapsule or granule shell or the microcapsule or granule matrix. In a further example, the one or more salts is mixed with the disintegrated plant material such as tobacco or non-tobacco plant fibres and also contained in the microcapsules or granules.
  • the one or more salts selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combinations thereof are believed to have a so-called salting in effect whereby the integrity of the particles containing a flavorant such as microcapsules or granules is maintained until the salt concentration is lowered.
  • the one or more salts of the oral smokeless moist snuff composition and/or the oral smokeless moist snuff product includes the sodium chloride and/or the potassium chloride occurring naturally in the disintegrated plant material.
  • the one or more salts of the oral smokeless moist snuff composition and/or the oral smokeless moist snuff product includes added salts as well as sodium chloride and/or potassium chloride occurring naturally in the disintegrated plant material.
  • the one or more salts described herein includes salts commonly used in snuff, such as sodium chloride, as well as salts used as pH adjusters, such as sodium carbonate.
  • Sodium chloride provides a salty taste and/or antimicrobial activity and may also influence the cellulose-derivatized polymer cloud point.
  • Sodium carbonate provides pH adjustment and may also influence the cellulose-derivatized polymer cloud point.
  • the one or more salts may provide taste, pH adjustment, antimicrobial activity etc.
  • the one or more salts may be sodium lactate and/or potassium lactate.
  • sodium lactate and/or potassium lactate have a neutral taste, an antibacterial activity and are also believed to have a lower impact on a cellulose- derivatized polymer than, for instance, sodium chloride.
  • all or at least part of the sodium chloride may be exchanged for sodium lactate and/or potassium lactate.
  • the one or more salts may be selected from the group consisting of sodium chloride, potassium carbonate, potassium sulphate and any combinations thereof.
  • the one or more salts may comprise sodium carbonate and a salt selected from the group consisting of potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combination thereof.
  • the one or more salts may comprise potassium carbonate and a salt selected from the group consisting of sodium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combination thereof.
  • the one or more salts of the oral smokeless moist snuff product described herein may comprise or consist of sodium chloride, sodium carbonate and potassium sulphate.
  • the ratio sodium chloride: sodium carbonate: potassium sulphate may be about 6:3:1 or about 7:2:1 . It will be appreciated that the potassium sulphate may be replaced entirely or partly with sodium chloride and/or potassium chloride.
  • the one or more salts of the oral smokeless moist snuff product described herein may comprise or consist of sodium carbonate and sodium chloride and/or potassium chloride.
  • the one or more salts of the oral smokeless moist snuff product described herein may comprise or consist of sodium chloride, sodium carbonate and optionally one or more salts selected from the group consisting of potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combinations thereof.
  • the one or more salts of the oral smokeless moist snuff product described herein may comprise or consist of sodium sulphate and/or potassium sulphate and/or one or more salts selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate and any combinations thereof.
  • the total amount of the one or more salts of the oral smokeless moist snuff composition and/or the oral smokeless moist snuff product prepared for the consumer may be estimated using any method known in the art to a skilled person. For instance, the total amount of the one or more salts may be estimated or indicated based on the
  • the amount of the one or more salts will depend on the total amount of moisture of the oral smokeless moist snuff composition. Generally, to maintain flavorant particle integrity in the oral smokeless moist snuff product the amount of the one or more salts will have to be increased when the total amount of moisture of the oral smokeless moist snuff composition is raised.
  • the inventors of the present disclosure have found that for a total amount of moisture within the range of from about 35% by weight to about 60% by weight based on the total weight of the oral smokeless moist snuff composition, the total amount of the one or more salts should be within the range of about 15 % by weight to about 35 % by weight based on the total weight of water and total weight of the one or more salts in the oral smokeless moist snuff composition.
  • the amount of particles containing a flavorant as described herein may be within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the amount of particles containing a flavorant may be within the range of from about 5 % by weight to about 25 % by weight, from about 5% by weight to about 20 % by weight, from about 5 % by weight to about 15 % by weight, from about 5 % by weight to about 10 % by weight or from about 10 % by weight to about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the amount of particles containing a flavorant may be about 5 % by weight, about 10 % by weight, about 15 % by weight or about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the total amount of the one or more salts may be within the range of from about 15 % by weight to about 35 % by weight, from about 15 % by weight to about 25 % by weight or from about 20 % by weight to about 25 % by weight, based on the total weight of water and the total weight of the one or more salts of the oral smokeless moist snuff composition, and the total amount of moisture may be within the range of from about 45 % by weight to about 60 % by weight based on the total weight of the oral smokeless moist snuff composition.
  • the amount of particles containing a flavorant as described herein may be within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the amount of particles containing a flavorant may be within the range of from about 5 % by weight to about 25 % by weight, from about 5% by weight to about 20 % by weight, from about 5 % by weight to about 15 % by weight, from about 5 % by weight to about 10 % by weight or from about 10 % by weight to about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the amount of particles containing a flavorant may be about 5 % by weight, about 10 % by weight, about 15 % by weight or about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the total amount of the one or more salts may be within the range of from about 15 % by weight to about 35 % by weight, from about 15 % by weight to about 25 % by weight or from about 20 % by weight to about 25 % by weight, based on the total weight of water and the total weight of the one or more salts of the oral smokeless moist snuff composition, and the total amount of moisture may be within the range of about 33 % by weight to about 37 % by weight such as about 35 % by weight based on the total weight of the oral smokeless moist snuff composition.
  • the amount of particles containing a flavorant as described herein may be within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the amount of particles containing a flavorant may be within the range of from about 5 % by weight to about 25 % by weight, from about 5% by weight to about 20 % by weight, from about 5 % by weight to about 15 % by weight, from about 5 % by weight to about 10 % by weight or from about 10 % by weight to about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the amount of particles containing a flavorant may be about 5 % by weight, about 10 % by weight, about 15 % by weight or about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the total amount of the one or more salts may be within the range of from about 15 % by weight to about 35 % by weight, from about 15 % by weight to about 25 % by weight or from about 20 % by weight to about 25 % by weight, based on the total weight of water and the total weight of the one or more salts of the oral smokeless moist snuff composition, and the total amount of moisture may be within the range of about 38 % by weight to about 42 % by weight such as about 40 % by weight based on the total weight of the oral smokeless moist snuff composition.
  • the amount of particles containing a flavorant as described herein may be within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the amount of particles containing a flavorant may be within the range of from about 5 % by weight to about 25 % by weight, from about 5% by weight to about 20 % by weight, from about 5 % by weight to about 15 % by weight, from about 5 % by weight to about 10 % by weight or from about 10 % by weight to about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the amount of particles containing a flavorant may be about 5 % by weight, about 10 % by weight, about 15 % by weight or about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the total amount of the one or more salts may be within the range of from about 15 % by weight to about 35 % by weight, from about 15 % by weight to about 25 % by weight or from about 20 % by weight to about 25 % by weight, based on the total weight of water and the total weight of the one or more salts of the oral smokeless moist snuff composition, and the total amount of moisture may be within the range of about 43% by weight to about 47 % by weight such as about 45 % by weight based on the total weight of the oral smokeless moist snuff composition.
  • the amount of particles containing a flavorant as described herein may be within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the amount of particles containing a flavorant may be within the range of from about 5 % by weight to about 25 % by weight, from about 5% by weight to about 20 % by weight, from about 5 % by weight to about 15 % by weight, from about 5 % by weight to about 10 % by weight or from about 10 % by weight to about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the amount of particles containing a flavorant may be about 5 % by weight, about 10 % by weight, about 15 % by weight or about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the total amount of the one or more salts may be within the range of from about 15 % by weight to about 35 % by weight, from about 15 % by weight to about 25 % by weight or from about 20 % by weight to about 25 % by weight, based on the total weight of water and the total weight of the one or more salts of the oral smokeless moist snuff composition, and the total amount of moisture may be within the range of about 48 % by weight to about 52 % by weight such as about 50 % by weight based on the total weight of the oral smokeless moist snuff composition.
  • the amount of particles containing a flavorant as described herein may be within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the amount of particles containing a flavorant may be within the range of from about 5 % by weight to about 25 % by weight, from about 5% by weight to about 20 % by weight, from about 5 % by weight to about 15 % by weight, from about 5 % by weight to about 10 % by weight or from about 10 % by weight to about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the amount of particles containing a flavorant may be about 5 % by weight, about 10 % by weight, about 15 % by weight or about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the total amount of the one or more salts may be within the range of from about 15 % by weight to about 35 % by weight, from about 15 % by weight to about 25 % by weight or from about 20 % by weight to about 25 % by weight, based on the total weight of water and the total weight of the one or more salts of the oral smokeless moist snuff composition, and the total amount of moisture may be within the range of about 53 % by weight to about 57 % by weight such as about 55 % by weight based on the total weight of the oral smokeless moist snuff composition.
  • the amount of particles containing a flavorant as described herein may be within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the amount of particles containing a flavorant may be within the range of from about 5 % by weight to about 25 % by weight, from about 5% by weight to about 20 % by weight, from about 5 % by weight to about 15 % by weight, from about 5 % by weight to about 10 % by weight or from about 10 % by weight to about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the amount of particles containing a flavorant may be about 5 % by weight, about 10 % by weight, about 15 % by weight or about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the total amount of the one or more salts may be within the range of from about 15 % by weight to about 35 % by weight, from about 15 % by weight to about 25 % by weight or from about 20 % by weight to about 25 % by weight, based on the total weight of water and the total weight of the one or more salts of the oral smokeless moist snuff composition, and the total amount of moisture may be within the range of about 58 % by weight to about 62 % by weight such as about 60 % by weight based on the total weight of the oral smokeless moist snuff composition.
  • the amount of particles containing a flavorant as described herein may be within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the amount of particles containing a flavorant may be within the range of from about 5 % by weight to about 25 % by weight, from about 5% by weight to about 20 % by weight, from about 5 % by weight to about 15 % by weight, from about 5 % by weight to about 10 % by weight or from about 10 % by weight to about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
  • the amount of particles containing a flavorant may be about 5 % by weight, about 10 % by weight, about 15 % by weight or about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
  • an oral smokeless moist snuff product comprising: (a) an oral smokeless moist snuff composition comprising:
  • the total amount of the one or more salts is about 25 % by weight based on the total weight of water and total weight of the one or more salts in the oral moist smokeless snuff composition
  • the total amount of moisture is about 46 % by weight based on the total weight of the oral smokeless moist snuff composition
  • the oral smokeless moist snuff product may comprise from about 1 to about 5 % by weight, such as from about 2 to about 4 % by weight, based on the dry weight of the oral smokeless moist snuff composition, of a humectant selected from the group consisting of propylene glycol and glycerol.
  • the oral smokeless moist snuff product described herein may comprise no or substantially no humectant.
  • the humectant should be selected in such a way and/or in an amount that it influences the cloud point of the cellulose-derivatized polymer to only a small extent or not at all. For instance, glycerol will have only a small impact on the cellulose polymer cloud point whereas propylene glycol will have a larger impact. Therefore, in case propylene glycol is used the amount should be adjusted to avoid a too large impact on the cellulose cloud point.
  • propylene glycol in an amount of about 2 to about 4 % by weight such as from about 0.5 to about 2 % by weight, such as from about 1 to about 3 % by weight, such as from about 1 to about 2 % by weight, based on the dry weight of the oral smokeless moist snuff composition, may be added to the oral smokeless moist snuff product described herein.
  • the impact of the humectant on the cellulose-derivatized polymer cloud point may at least to some extent be compensated for by increasing the amount of the one or more salts.
  • the humectant of the oral smokeless moist snuff product described herein may contain a humectant comprising or consisting of glycerol.
  • total amount of moisture refers to the total amount of oven volatile ingredients, such as water and other oven volatiles (e.g. propylene glycol, ethanol etc.) in the preparation, composition or product referred to.
  • the total amount of moisture is given herein as percent by weight (wt%) of the total weight of the preparation, composition or product referred to.
  • the total amount of moisture as referred to herein may be determined by using the LOD method disclosed in the Examples in which the oven volatile content at a temperature of about 105°C is determined.
  • the total amount of moisture may refer to the total amount of oven volatiles measured of a temperature at about 105°C, such as measured with an LOD method.
  • the total amount of moisture of the oral smokeless moist snuff composition may range from about 35 % by weight to about 60 % by weight such as from about 40 % by weight to about 60 % by weight, from about 45 % by weight to about 60 % by weight, from about 45 % by weight to about 55 % by weight, from about 50 % by weight to about 55 % by weight, from about 50 % by weight to about 60 % by weight or from about 55 % by weight to about 60 % by weight.
  • the total amount of moisture of the oral smokeless moist snuff composition may be about 35 % by weight, about 40% by weight, about 45 % by weight, about 46 % by weight, about 55 % by weight or about 60 % by weight.
  • the water content of the oral smokeless moist snuff composition and/or the oral smokeless moist snuff product includes all water present such as added water and water occurring naturally in the disintegrated plant material.
  • an oral smokeless moist snuff product as described herein wherein the total amount of moisture of the oral smokeless moist snuff composition is about 40 % by weight.
  • the one or more salts comprises or consists of sodium chloride, sodium carbonate and potassium sulphate.
  • the ratio sodium chloride: sodium carbonate: potassium sulphate may be about 6:3:1 or about 7:2:1.
  • an oral smokeless moist snuff product as described herein wherein the total amount of moisture of the oral smokeless moist snuff composition is about 46 % by weight, and the one or more salts may comprise or consist of sodium chloride, sodium carbonate and potassium sulphate. The ratio sodium chloride: sodium carbonate: potassium sulphate may be about 7:2:1.
  • an oral smokeless moist snuff product as described herein wherein the total amount of moisture of the oral smokeless moist snuff composition is about 55 % by weight, and the one or more salts may comprise or consist of sodium chloride, sodium carbonate and potassium sulphate. The ratio sodium chloride: sodium carbonate: potassium sulphate may be about 7:2:1.
  • an oral smokeless moist snuff product as described herein wherein the total amount of moisture is about 35 wt%, and the one or more salts may comprise or consist of sodium chloride and sodium carbonate.
  • the ratio sodium chloride: sodium carbonate may be about 3:1.
  • an oral smokeless moist snuff product as described herein wherein the total amount of moisture of the oral smokeless moist snuff composition is about 46 wt%, and the one or more salts may comprise or consist of sodium chloride and sodium carbonate.
  • the ratio sodium chloride: sodium carbonate may be about 3:1 or about 4:1 .
  • an oral smokeless moist snuff product as described herein wherein the total amount of moisture is about 55 wt% of the oral smokeless moist snuff composition, and the one or more salts may comprise or consist of sodium chloride and sodium carbonate.
  • the ratio sodium chloride: sodium carbonate may be about 4:1.
  • the particles described herein may be microparticles, such as microcapsules or granules as described herein.
  • the particles may or may not contain a carrier.
  • the particles such as microcapsules or granules of the present disclosure contain a flavorant.
  • a flavorant As used herein, the terms “flavorant”, “flavor” “flavoring agent” or the like denote a substance used to influence the aroma and/or taste of the oral smokeless moist snuff product.
  • the flavorant may be a single flavor or a combination of flavorants/flavors.
  • the flavorant may be in solid or liquid form.
  • the liquid form may be a liquid composition such an oil.
  • the flavorant may be an essential oil, a compounded flavoring and/or extracts. Further, the flavorant may be natural or synthetic.
  • flavorants include menthol, peppermint, spearmint, liquorice, anethol, geranium, lemon oil, orange oil, grapefruit oil, bergamot oil, vanilla, coffee, coconut, almond, pecan, walnut, peanut, hazelnut, ginger, fennel, clove, anise, cardamom, coriander, basil, oregano, rosemary, thyme, sage, jasmine, lavender, wintergreen, cocoa and cumarin.
  • the flavor may contain tobacco flavorant.
  • the flavorant may be a non-tobacco flavorant.
  • the flavorant may be a solid encapsulated by a shell such as a coating comprising, for instance, hydroxypropyl methylcellulose, to provide a granule or microcapsule.
  • the flavorant may be dispersed within a matrix and optionally encapsulated by a shell such as a coating comprising, for instance,
  • hydroxypropyl methylcellulose to provide a granule or microcapsule.
  • the particles containing a flavorant such as microcapsules may be a mixture of microcapsules containing different flavorants. For instance, 50% of the microcapsules may contain a first flavorant and the remaining 50% may contain a second flavorant different from the first flavorant.
  • the inner coating and/or the outer coating of the microcapsules may or may not contain a flavor.
  • the inner and/or the outer coating contain no flavor.
  • the inner and/or outer contain a non-tobacco flavor.
  • the total weight of the particles containing a flavorant such as microcapsules contained within the oral smokeless moist snuff product may vary.
  • the amount of said particles may be within the range of from about 1 % by weight to about 25 % by weight , such as from about 5 % by weight to about 25 % by weight or from about 5 % by weight to about 10 % by weight, based on the total weight of the oral smokeless moist snuff product.
  • the amount of said particles may be about 5 % by weight, about 10 % by weight, about 15 % by weight or about 20 % by weight.
  • the amount of said particles may be about 10 % by weight.
  • the particles such as microcapsules or granules, containing a flavorant may be mixed with an oral smokeless moist snuff composition to provide the oral smokeless moist snuff product.
  • the particles containing a flavorant may be added to the oral smokeless moist snuff composition or vice versa.
  • the particles containing a flavorant and the components of the oral smokeless moist snuff composition may be mixed in any order to provide the oral smokeless moist snuff product.
  • a single particle such as a capsule or granule having a size larger than that of the microcapsules or granules may be used in addition to or instead of a plurality of microcapsules and/or granules.
  • the single capsule may contain a flavorant that is the same as or different from that of the microcapsules and/or granules.
  • the shape of the particles may vary, but typically the microcapsules or granules have a substantially spherical shape. Alternatively, the microcapsules or granules may have other types of shapes such as rectilinear, oblong, elliptical or oval shapes.
  • the particles containing a flavorant such as microcapsules or granules may be uniform or varied in size.
  • the microcapsule or granule diameter may be from 1 to 5 mm, such as from 1 to 4 mm or from 1 to 3 mm or from 300 micrometers to 1 mm.
  • the microcapsules or granules may be spherical and have a diameter equal to or less than about 300 micrometers, such as from 100-300 micrometers, such as from 100-200 micrometers, or from 1 to 40 micrometers or from 1 to 20 micrometers.
  • the microcapsule or granule diameter may be about 1 mm.
  • microcapsules or granules of substantially uniform size In some oral smokeless moist snuff products it may be desired to include microcapsules or granules of substantially uniform size, whereas in other oral smokeless moist snuff products it may be desired to include microcapsules or granules with varying size.
  • particles such as microcapsules of different sizes and types may be included in the oral smokeless moist snuff products to provide for a desired flavor release profile.
  • a first flavorant may be released from a first set of microcapsules or granules
  • a second flavorant may be released from a second set of microcapsules or granules.
  • the release of the first flavorant may take place prior to, at the same time as or after release of the second flavorant.
  • the particles containing a flavorant described herein may be dyed.
  • the dye may be provided by a color additive approved for use in food. By providing at least part of the particles as dyed particles the consumer may perceive the oral smokeless moist snuff product as more interesting and/or appealing.
  • the crush strength of the microcapsules disclosed herein is sufficient to allow for normal handling and storage without significant premature or undesirable breakage.
  • a non-encapsulated flavorant may be mixed with the disintegrated plant material such as tobacco or non-tobacco plant fibres of the oral smokeless moist snuff product described herein.
  • the flavorant may be added by spraying it onto the tobacco or the non-tobacco plant fibres.
  • the flavorant may be sprayed directly onto loose tobacco and/or non-tobacco fibres or onto pouches containing tobacco and/or non- tobacco fibres. In this way, a user placing the oral smokeless moist snuff product described herein into his or her mouth will immediately experience the flavorant mixed with the tobacco or non-tobacco plant fibres and then gradually also experience the flavorant released from the microcapsules.
  • the non-encapsulated flavorant may be the same or different from that contained in the particles containing a flavorant such as microcapsules or granules. In this way, a consumer may perceive the taste of the oral smokeless moist snuff product to evolve and/or change over time.
  • a non-encapsulated flavorant may be added to the oral smokeless moist snuff product described herein by coating at least part of one inside surface, such as an inside lid or bottom surface, of a container with the flavorant, adding the oral smokeless moist snuff product to the container and closing of the container.
  • the container may be a packaging container for an oral smokeless moist snuff product. When the container is closed, the flavorant applied to the at least part of one inside surface of the container will flavorize the oral smokeless moist snuff product. Accordingly, there is provided a method for adding a flavorant to an oral smokeless moist snuff product as described herein, said method comprising the steps of:
  • the container for an oral smokeless moist snuff product does not form part of the oral smokeless moist snuff product described herein.
  • the overall result for a user may be a constant flavor intensity, an increase in flavor intensity over a certain time, a change in flavour etc.
  • the oral smokeless moist snuff product may further comprise a sweetener. Suitable sweeteners include natural sweeteners such as fructose, sucrose, glucose, maltose, mannose, galactose, lactose or xylitol.
  • the sweetener may also be an artificial sweetener such as sucralose, saccharin, aspartame, acesulfame K, neotam or stevia.
  • the sweetener may be mixed with the oral smokelss moist snuff composition and/or be provided in encapsulated form.
  • a pH adjusting agent may be included in the oral smokeless moist snuff product described herein to provide a desired pH value.
  • the pH adjusting agent may be an alkali metal base or an acid.
  • the alkali metal base may be sodium hydroxide or potassium hydroxide.
  • the acid may be acetic acid, lactic acid or citric acid.
  • the pH adjusting agent may be mixed with the oral smokelss moist snuff composition and/or be provided in encapsulated form.
  • a buffering agent may be present in the oral smokeless moist snuff product described herein in order to maintain pH close to a desired value.
  • Suitable buffering agents include alkali metal carbonates and alkali metal bicarbonates.
  • the alkali metal carbonates may be sodium carbonate or potassium carbonate.
  • the alkali metal bicarbonates may be sodium bicarbonate or potassium bicarbonate.
  • the buffering agent may be mixed with the oral smokelss moist snuff composition and/or be present in encapsulated form.
  • the oral smokeless moist snuff described herein may also include additives such as disintegration aids, antioxidants, binders, colorants, fillers, thickening agents and/or combinations thereof.
  • the additives may be mixed with the oral smokelss moist snuff composition and/or be present in encapsulated form or in non-encapsulated form.
  • the particles described herein such as microcapsules or granules may be manufactured by coating a gelatine microcapsule with a cellulose polymer such as hydroxypropyl methylcellulose using fluidized bed technique. However, any other technique known in the art to the skilled person may be used.
  • the oral smokeless moist snuff product described herein may be manufactured by dispersing the microcapsules with the other components of the oral smokeless moist snuff.
  • an oral smokeless moist snuff product comprising: a) from 14 to 66 wt% of disintegrated plant material, b) from 0.5 to 20 wt% of microcapsules comprising a flavorant encapsulated by a cellulose polymer selected from the group consisting hydroxypropyl methylcellulose, hydroxypropyl cellulose, methyl cellulose and any combination thereof, c) from 1 .5 to 18 wt% of salt selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combination thereof, wherein the moisture content of the product is within the range of from 30 to 60 wt%.
  • particulate is used for a particle size of the product which enables the final product to be provided in so-called loose form, from which a pinch of snus may be made in individual sized by a user of a product.
  • oral or “oral use” refer to use in the oral cavity, i.e. for chewing purposes or buccal placement.
  • LOD Loss On Drying and is a method to measure the loss of weight of the sample when dried at 105°C. The sample is dried until the sample weight is substantially constant. The LOD method is described in the Examples section.
  • wt% stands for weight% means weight percent in the composition or product referred to.
  • wt% weight%
  • weight% weight percent in the composition or product referred to.
  • % weight percent
  • HPMC is an abbreviation for hydroxypropyl methylcellulose.
  • rpm revolutions per minute
  • GC Gas Chromatography
  • MS Mass Spectroscopy
  • GCMS Gas Chromatography Mass Spectroscopy
  • w/w weight by weight.
  • Figure 1 shows a graph indicating flavor intensity experienced by eleven test persons during a time period of 60 minutes.
  • Headspace screw top vials (20 ml) were purchased from ThermoScientific. Petroleum ether Suprasolv was purchased from VWR. Samples were shaken on an incubation orbital shaker, professional 3500, purchased from VWR. Analyses were performed on an Agilent 5890/5972/7673 GCMS-system, operating in full scan mode. GC column was an Agilent Innowax (60 m x 0.25 mm x 0.25 urn).
  • total flavor intends the total analyzed amount of flavor in the product consisting of moist snus and microcapsules.
  • the total flavor intends the sum of the flavor of the microcapsules and the flavor contained in the moist snus.
  • free flavor intends the analyzed amount of flavor in the moist snus.
  • the free flavor intends the flavor contained in the moist snus, excluding the flavor of the non-disintegrated microcapsules.
  • the flavor is a mixture of peppermint and menthol.
  • a GC/MS method (the same method for both extractions) was used to estimate the amount of flavor in the extracts. This was a semi-quantitative method for menthol, which served as a marker for all flavor compounds. The area of menthol was integrated and area units were compared between samples.
  • grinded and heated moist tobacco refers to tobacco that has been prepared as follows.
  • the tobacco was grinded and pasteurized, and the moisture content was adjusted with water to about 35 wt%.
  • the chloride content of the tobacco flour prior to grinding and pasteurization i.e. the sum of chloride from NaCI and KCI, was about 3. wt% based on the weight of the tobacco flour.
  • the total amount of moisture of the tobacco flour was 7 wt%.
  • “moist snus” refers to a mixture of grinded and heated moist tobacco, sodium carbonate, potassium sulphate, sodium chloride, ethanol and water. In some examples the potassium sulphate was excluded.
  • “moist snus product” refers to the mixture resulting from adding microcapsules to the moist snus, i.e. a mixture of microcapsules, grinded and heated moist tobacco, sodium carbonate, potassium sulphate, sodium chloride, ethanol and water. In some examples the potassium sulphate was excluded. LOP method
  • the moisture content of each of the tobacco material and the non-tobacco plant fibers, if present, was determined by using a method based on literature references Federal Register/ vol.74, no. 4/712-719/Wednesday, January 7, 2009/Notices, "Total moisture determination” and AOAC (Association of Official Analytical Chemics), Official Methods of Analysis 966.02: “Moisture in Tobacco” (1990), Fifth Edition, K. Helrich (ed).
  • the oven volatile (OV) content of the tobacco material and the non-tobacco plant fibers, if present, is measured as described
  • Mettler Toledo's Moisture Analyzer HB43 a balance with halogen heating technology, was used (instead of an oven and a balance as in the mentioned literature references).
  • the sample was heated to 105 °C (instead of 99.5 ⁇ 0.5 °C as in the mentioned literature references).
  • the measurement was stopped when the weight change was less than 1 mg during a 90 seconds time period.
  • the moisture content (i.e. oven volatile content) as weight percent of the original weight of the sample is then calculated automatically by the Moisture Analyzer HB43.
  • the content of oven volatiles other than water (i.e. nonaqueous oven volatiles) in tobacco flour is normally less than 1 % by weight. Therefore the moisture content of tobacco material as measured using the herein described method substantially corresponds to the actual water content of the tobacco material.
  • the given water content of the initial tobacco preparations is the calculated sum of oven volatiles content of the tobacco material and the non-tobacco plant fibers if present, as measured by the above disclosed method, and, where applicable, the amount of water added to the tobacco material in the process.
  • Microcapsules were formed in the following manner.
  • a fluid bed Mini-Glatt (from Glatt GmbH, Binzen) with bottom spray coating (Wurster) was used.
  • the spray nozzle was 0.5 mm in diameter.
  • the bottom filter was 100 ⁇ , mounted on a bottom plate with diameter 7.5 cm.
  • Millicaps 1000 E_1413279 from V. MANE FILS, France
  • the Millicaps were substantially gelatin microcapsules containing a liquid
  • the moist snus was prepared by mixing sodium carbonate, potassium sulphate, sodium chloride, ethanol and water with grinded and heated moist tobacco. The amounts were as indicated in Table 2 below.
  • the moist snus of the moist snus product consisted of grinded and heated moist tobacco prepared as described above, sodium carbonate, potassium sulphate, sodium chloride, ethanol and water in amounts as indicated in Table 2.
  • the above manufactured microcapsules were mixed with the moist snus, said moist snus having a total amount of moisture of about 46 % by weight based on the moist snus, to provide a moist snus product.
  • the composition of the moist snus product is indicated in Table 2.
  • the moist snus product was packaged in pouches, each pouch having with a weight of about 0.8 g.
  • the pouches were stored in a sealed plastic bag for two weeks at room temperature.
  • Pouches consisting of the moist snus and microcapsules, said pouches being
  • Example 1 manufactured as in Example 1 , were evaluated regarding flavor release function as follows. The pouches were stored for two weeks in a sealed plastic bag prior to use.
  • test persons used the pouches for 60 minutes.
  • the pouch was put between the gum and the upper lip and the pouch was fixed in that position during the whole test period.
  • the total amount of menthol left in the used pouches were analyzed and compared to the total amount of analyzed menthol in unused pouches.
  • the test persons used two pouches each.
  • the pouches were analyzed using GC/MS according to the method described above. The results are indicated in Table 4 (Total flavor of unused pouches) and Table 5 (Total flavor of used pouches).
  • the microcapsule flavorant was peppermint and menthol. The analysis was performed with respect to menthol.
  • Millicaps 1000 E_1413279 were purchased from V. MANE FILS, France.
  • the Millicaps were substantially gelatin microcapsules containing a liquid menthol flavorant.
  • Moist snus was prepared by mixing sodium carbonate, potassium sulphate, sodium chloride, ethanol and water with grinded and heated moist tobacco. The amounts were as indicated in Table 6 below.
  • the moist snus of the moist snus product consisted of grinded and heated moist tobacco, sodium carbonate, potassium sulphate, sodium chloride, ethanol and water in amounts as indicated in Table 6.
  • the Millicaps were mixed with the moist snus, said moist snus having a total amount of moisture of about 46 % by weight based on said moist snus, to provide a moist snus product.
  • the composition of the moist snus product was as indicated in Table 6.
  • the moist snus product was packaged in pouches, each pouch having a weight of about 0.8 g. 10 pouches were prepared.
  • the pouches were stored for two weeks at room temperature in a sealed plastic bag.
  • Moist snus was prepared by mixing sodium carbonate, potassium sulphate, sodium chloride, ethanol and water with grinded and heated moist tobacco. The amounts were as indicated in Table 8 below. The total amount of moisture of the moist snus was about 45 % by weight based on said moist snus.
  • the mixture was then stored in a sealed test tube in room temperature for two weeks.
  • the composition of the moist snus product was as indicated in Table 8.
  • the free flavor content of the stored Sample 1 was only 3% indicating that substantially no flavor release from the microcapsules had taken place.
  • the free flavor content of the stored Sample 2 was 42% indicating a significant flavor release from the microcapsules.
  • Microcapsules were formed in the following manner.
  • Millicaps 1000E_1413279 from V. MANE FILS, France
  • the Millicaps were substantially gelatin microcapsules containing a liquid peppermint/menthol flavorant.
  • the above prepared 230 g weight suspension with talc and dissolved hydroxypropyl methylcellulose was then sprayed on to the Millicaps
  • the formed microcapsules were then sieved through a sieve with a mesh size of 2 mm and the upper fraction was removed.
  • the moist snus was prepared as in example 1 .
  • the total amount of moisture of the snus was about 46 % by weight based on said moist snuff.
  • the above manufactured microcapsules were mixed with the moist snus.
  • the composition of the moist product is indicated in Table 2.
  • Moist snus was prepared by mixing sodium carbonate, ethanol and water with grinded and heated moist tobacco. The amounts were as indicated in Table 1 1 below. The total amount of moisture of the snus was about 46 % by weight based on said moist snus. Thus, the moist snus of the moist snus product consisted of grinded and heated moist tobacco prepared as described above, sodium carbonate, ethanol and water in amounts as indicated in Table 1 1.
  • Microcapsules manufactured as in Example 5 were mixed with the moist snus to provide a moist snus product.
  • the composition of the moist snus product is indicated in Table 1 1.
  • Moist snus was prepared by mixing sodium chloride, sodium carbonate, ethanol and water with grinded and heated moist tobacco. The amounts were as indicated in Table 13 below. The total amount of moisture of the snus was about 46 % by weight based on said moist snus.
  • the moist snus of the moist snus product consisted of grinded and heated moist tobacco prepared as described above, sodium chloride, sodium carbonate, ethanol and water in amounts as indicated in Table 13.
  • Microcapsules manufactured as in Example 5 were mixed with the moist snus to provide a moist snus product.
  • the composition of the moist snus product is indicated in Table 13.
  • Moist snus was prepared by mixing sodium chloride, sodium carbonate, ethanol and water with grinded and heated moist tobacco. The amounts were as indicated in Table 15 below. The total amount of moisture of the snus was about 46 % by weight based on said moist snus.
  • the moist snus of the moist snus product consisted of grinded and heated moist tobacco prepared as described above, sodium chloride, sodium carbonate, ethanol and water in amounts as indicated in Table 15.
  • Microcapsules manufactured as in Example 5 were mixed with the moist snus to provide a moist snus product.
  • the composition of the moist snus product is indicated in Table 15. Table 15
  • Moist snus was prepared by mixing sodium carbonate, sodium chloride, potassium sulphate, propylene glycole, ethanol and water with grinded and heated moist tobacco. The amounts were as indicated in Table 17 below. The total amount of moisture of the snus was about 46 % by weight based on said moist snus.
  • the moist snus of the moist snus product consisted of grinded and heated moist tobacco prepared as described above, sodium carbonate, sodium chloride, potassium sulphate, propylene glycole, ethanol and water in amounts as indicated in Table 17.
  • Microcapsules manufactured as in Example 5 were mixed with the moist snus to provide a moist snus product.
  • the composition of the moist snus product is indicated in Table 17. Table 17
  • the above moist product consisting of moist snus and microcapsules were evaluated regarding chemical storage stability as follows. Analysis regarding content of menthol was performed in two batches, one for free flavor and one for total flavor. As indicated in table 18, the free flavor content of the moist snus was only 5.3% after storage 2 weeks in room temperature. It can be concluded that the HPMC-talc coated gelatin microcapsules containing the liquid flavorant did not release the flavorant to any significant extent. Thus, the HPMC-talc coated gelatin microcapsules containing the liquid flavorant are substantially storage stable in the moist snus.
  • the following method may be used to measure the conductivity of moist snus.
  • Equipment conductivity measurement apparatus, glass beaker and a magnetic stirrer.

Landscapes

  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Agronomy & Crop Science (AREA)
  • Botany (AREA)
  • Manufacture Of Tobacco Products (AREA)
  • Cosmetics (AREA)

Abstract

There is provided an oral smokeless moist snuff product comprising: (a) an oral smokeless moist snuff composition comprising: -disintegrated plant material, -one or more salts selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combination thereof, and -water, wherein the total amount of the one or more salts is within the range of from about 15 % by weight to about 35 % by weight based on the total weight of water and total weight of the one or more salts in the oral moist smokeless snuff composition, wherein the total amount of moisture is within the range of from about 35 % by weight to about 60 % by weight based on the total weight of the oral smokeless moist snuff composition; (b) particles comprising a flavorant and a cellulose-derivatized polymer selected from the group consisting of hydroxypropyl methylcellulose, hydroxypropyl cellulose, methyl cellulose and any combination thereof, wherein the amount of said particles is within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product.

Description

AN ORAL SMOKELESS MOIST SNUFF PRODUCT
TECHNICAL FIELD
The present disclosure relates to oral smokeless moist snuff products containing particles, such as microparticles, for flavor release. The disclosure also relates to methods for making such products and uses thereof.
BACKGROUND
Smokeless tobacco for oral use includes chewing tobacco, dry snuff and moist (wet) snuff. Generally, dry snuff has moisture content of less than 10 wt% and moist snuff has a moisture content of above 40 wt%. Semi-dry products having between 10% to 40 wt% moisture content are also available.
Smokeless tobacco products for oral use are made from tobacco leaves, such as lamina and stem of the tobacco leaf. The material from roots and stalks are normally not utilized for production of smokeless tobacco compositions for oral use.
There are two types of moist snuff, the American type and the Scandinavian type.
American-type moist snuff is available in a loose form or as pre-packed pouches and is typically used between the lower gum and lip. The use of American-type moist snuff is commonly called dipping. Snus is the Scandinavian-type of moist snuff which is also available in loose form or as pre-packed portions in pouches. Snus is typically used between the upper gum and lip.
American-type moist snuff is commonly produced through a fermentation process of moisturized ground or cut tobacco. Scandinavian-type moist snuff (snus) is commonly produced by using a heat-treatment process (pasteurization) instead of fermentation. The heat-treatment is carried out in order to degrade, destroy or denature at least a portion of the microorganisms within the tobacco preparation. In production processes typically used today for producing pouched snus products, the tobacco preparation subjected to this heat-treatment process normally has moisture content within the range of from about 22 to 44% w/w. Generally, additional water, salt, pH adjuster and additional ingredients, such as flavours, are added to the tobacco preparation after this heat-treatment in order to provide the final smokeless tobacco composition, such as the moist snuff.
The main ingredients of oral smokeless moist snuff are tobacco, water, sodium carbonate, sodium chloride and a humectant such as propylene glycol or glycerol. Often a flavorant is present to enhance the organoleptic experience by a consumer. Instead of tobacco, fibres of non-tobacco plant material may be used thereby providing an oral smokeless non- tobacco product.
There are a number of properties of the oral smokeless moist snuff that are very important for the end user. Among them, the organoleptic properties, such as texture, aroma, taste, form and package of the product are of high importance for the consumer. A way of changing and/or improving the sensory experience by a consumer is to add a flavorant to the tobacco material. For instance, the flavorant may be added by mixing it with the tobacco material. When the oral smokeless tobacco product is placed in a consumer's oral cavity the natural tobacco flavor and/or the added flavorant will be extracted by the consumer's saliva. The flavorant is extracted gradually. After a certain time, such as about one hour, the consumer usually perceives the taste as gone and therefore disposes the product. It would be desirable that the flavor intensity experienced by a consumer remained constant or increased during a certain time period. Alternatively or additionally, the flavorant may be added to the tobacco formulation in a form that physically separates it from the tobacco formulation. For instance, particles containing a flavorant may be added. The particles containing a flavorant may be provided as a capsule, such as a encapsulated. Disintegration of the capsule leads to flavor release. The capsules may be designed so that flavor release only takes place when certain conditions are fulfilled. For instance, the capsules may be temperature sensitive so that a certain temperature is required for capsule disintegration and concomitant flavor release. Further, encapsulation of the flavorant prevents it from interacting with the tobacco composition and/or the atmosphere in the container for the tobacco composition. Such interaction may lead to a different and/or deteriorated sensorial experience and have a negative impact on stability. The use of flavorant containing microcapsules in dry snuff is known. Commonly, the microcapsule shell comprises gelatine. During storage in a refrigerator or at room temperature (i.e. about 22 °C) the gelatine shell maintains its integrity and does not
5 release the flavorant. When a consumer places the dry snuff containing the microcapsules into the mouth the gelatine capsules disintegrate and the flavorant is released.
Use of encapsulated flavorants for flavorization of oral smokeless moist snuff products presents a particular challenge. One the one hand, the capsule material must maintain its 10 integrity and substantially withstand leakage of the enclosed flavorant when mixed and stored together with the moist tobacco composition. On the other hand, the capsule material should be able to disintegrate and provide controlled release of the flavorant when the oral smokeless moist snuff product is placed in a user's mouth.
15 US patent No. 7,810,507 discloses a smokeless tobacco product containing
microencapsulated flavorants. A list of outer wall or shell material of the microcapsules is mentioned, said list including inter alia gelatine and hydroxypropyl methylcellulose. It is stated that microencapsulated tobacco flavorants will provide extended release of the tobacco flavor under conditions of normal use of the smokeless tobacco product, such as
20 under conditions of 45% or greater moisture level, based on the total weight of the
smokeless tobacco product. Alternatively, they may lose their physical integrity when the smokeless tobacco product reaches a certain pH or a certain temperature.
US 2004/0180067 discloses a particle composition containing a continuous phase of 5- 25 95% organically soluble cellulosic material selected from the group consisting of ethyl cellulose and hydroxypropyl cellulose dissolved in 5-95% organic fragrance chemicals and organic flavor chemicals. It is stated that a particle formed of hydroxypropyl cellulose and flavor will not dissolve in an aqueous solution of 10% NaCI, although flavor chemicals will partition into the aqueous phase over time.
30
WO 2009/073190 discloses a fast-dissolving film for use as a platform for the delivery of material to the oral cavity, comprising a film forming agent, a plasticizing agent and a water-soluble agent. The material may be nicotine. The film may be edible and is fast- dissolving upon contact with water-based aqueous systems such as human saliva. WO2009/056609 discloses oral smokeless tobacco compositions comprising
encapsulated flavorants. The encapsulating agent is hydrophobic and poorly soluble in aqueous solutions. The release of the flavourant may be caused by alteration/degradation of the encapsulating agent with saliva and/or thermal degradation, e.g. melting of the encapsulation agent at a temperature present in the oral cavity.
US 2010/0282267 discloses an encapsulated flavorant for use with smokeless tobacco. The encapsulated flavorant comprises a core with a lipid-based coating that provides stability when in contact with tobacco, yet releases flavor over time when the product is used.
It is an object of the present disclosure to overcome or at least mitigate some of the problems associated with flavorization of oral smokeless moist snuff. Further, it is an object of the present disclosure to provide an oral smokeless moist snuff product exhibiting satisfactory storage stability, such as satisfactory storage stability with respect to flavor. It is also an object of the present disclosure to provide an oral smokeless moist snuff product with attractive flavor characteristics.
SUMMARY
There is provided an oral smokeless moist snuff product comprising:
(a) an oral smokeless moist snuff composition comprising:
- disintegrated plant material,
-one or more salts selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combination thereof, and
- water,
wherein the total amount of the one or more salts is within the range of from about 15 % by weight to about 35 % by weight based on the total weight of water and total weight of the one or more salts in the oral moist smokeless snuff composition, wherein the total amount of moisture is within the range of from about 35 % by weight to about 60 % by weight based on the total weight of the oral smokeless moist snuff composition;
(b) particles comprising a flavorant and a cellulose-derivatized polymer selected from the group consisting of hydroxypropyl methylcellulose, hydroxypropyl cellulose, methyl cellulose and any combination thereof,
wherein the amount of said particles is within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product.
Further, there is provided a method for adding a flavorant to an oral smokeless moist snuff product as described herein, said method comprising the steps of:
a)applying a flavorant onto at least part of one inside surface of a container for an oral smokeless moist snuff product,
b) placing the oral smokeless moist snuff product as described herein in the container, and
c) closing the container.
DESCRIPTION
In accordance with the present disclosure, there is provided an oral smokeless moist snuff product comprising:
(a) an oral smokeless moist snuff composition as described herein, and (b) particles comprising a flavorant and a cellulose-derivatized polymer selected from the group consisting of hydroxypropyl methylcellulose, hydroxypropyl cellulose, methyl cellulose and any combination thereof, said particles being as defined herein. Thus, the present disclosure provides an oral smokeless moist snuff product comprising:
(a) an oral smokeless moist snuff composition comprising:
- disintegrated plant material,
-one or more salts selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combination thereof, and
- water, wherein the total amount of the one or more salts is within the range of from about 15 % by weight to about 35 % by weight based on the total weight of water and total weight of the one or more salts in the oral moist smokeless snuff composition, wherein the total amount of moisture is within the range of from about 35 % by weight to about 60 % by weight based on the total weight of the oral smokeless moist snuff composition; (b) particles comprising a flavorant and a cellulose-derivatized polymer selected from the group consisting of hydroxypropyl methylcellulose, hydroxypropyl cellulose, methyl cellulose and any combination thereof,
wherein the amount of said particles is within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product.
The present disclosure is based on the finding that gelatine microcapsules containing a flavorant when in admixture with an oral smokeless moist snuff composition soften and/or disrupt upon storage even in the presence of a quite large amount of salt. As a
consequence, there is a leakage of flavorant into the oral smokeless moist snuff composition containing tobacco or the non-tobacco plant fibres and this has a negative impact on storage stability and/or the desired flavor profile of the product.
Producers, retailers and consumers of tobacco products desire tobacco products or non- tobacco products with satisfactory storage stability at temperatures commonly
encountered or used. Frequently, oral smokeless moist snuff products are stored in refrigerators or at room temperature making storage stability at temperatures within the range of from about 5 to about 25 °C important. However, in colder or warmer places storage stability at slightly lower or higher temperature may be desirable. For instance, storage at about 0°C or about 30-45°C may be important. Common storage times range from two weeks to six months.
Surprisingly, it has been found that the oral smokeless moist snuff product described herein exhibits attractive flavor characteristics while at the same time providing for satisfactory storage.
The flavor profile of the oral smokeless tobacco product described herein, such as the oral smokeless moist snuff product, is such that flavorant release substantially takes place after the oral smokeless tobacco product has been placed into a user's mouth. Thus, there is little or no leakage of flavorant from the particles containing a flavorant during storage and prior to placing the oral smokeless moist snuff product into a user's mouth.
Further, when in the oral cavity of a user the flavorant release may take place during an extended period of time such as about one hour. During the flavorant release, the flavor intensity experienced by a user may increase over time so that the experienced flavor intensity is higher at the end of usage than at the beginning. Alternatively, during flavorant release a user may experience the flavor intensity to be substantially constant. As used herein, storage stability refers to the ability of a product to substantially withstand alteration and/or degradation during storage. The product may be the oral smokeless moist snuff product described herein and/or the particles containing a flavorant described herein. For instance, the particles containing a flavorant are considered to be storage stable when they substantially maintain their integrity during storage. As an example, storage stability may refer to storage stability at about room temperature, i.e. about 20-25 °C such as about 22 °C, during about three weeks. In a further example, storage stability may refer to storage stability at about 5 °C during about twenty weeks.
An oral smokeless moist snuff product may be considered to be storage stable when at least about 75 %, such as about 80%, about 85%, about 90%, about 95% or about 100%, of the total flavor of the flavorant particles remains encapsulated. The total flavour intends the sum of the flavor of the particles containing a flavorant and the flavor contained in the oral smokeless moist snuff composition. The total flavor may be determined as described in the experimental section of this document.
While not wishing to be bound by any specific theory, it is believed that the one or more salts selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate and potassium lactate and any combinations thereof act by lowering the cloud point of the cellulose-derivatized polymer enclosing the flavorant. In this document, the polymer cloud point defines the temperature above which the cellulose-derivatized polymer is insoluble, and below which it is soluble. By lowering the cloud point temperature, the particles containing a flavorant such as the microcapsules or granules maintain their integrity and thus their storage stability at a desired temperature thereby preventing or minimizing flavorant leakage during storage and prior to use. For instance, it may be desired that the particles such as the microcapsules or granules maintain their integrity at a temperature from about 0 °C to about 50°C, such as from about 5 °C to about 45°C or at body temperature (i.e. about 37°C). However, when the concentration of the one or more salts is lowered the particles such as the microcapsules or granules soften and/or disintegrate thereby releasing the encapsulated flavorant. Therefore, when the oral smokeless moist snuff product described herein is placed in a user's mouth saliva excretion lowers the salt concentration leading to microcapsule softening and disintegration followed by extended flavorant release. This is in contrast to, for example, thermosensitive microcapsules in which a mere temperature change results in capsule disintegration.
The salting out of polymers leading to polymer cloud point lowering is known in other technical fields. However, in oral smokeless moist snuff products the tobacco or the non- tobacco plant fibres contain a large number of components which may influence the polymer cloud point. Further, other components that are frequently present in oral smokeless moist snuff may also have an impact on the cellulose-derivatized polymer cloud point. It is therefore a complex task to provide an oral smokeless moist snuff product wherein extended flavor release substantially takes place after having placed the product into a user's mouth. The disintegrated plant material may be disintegrated tobacco or disintegrated non- tobacco plant fibres as described herein.
As used herein, the term "disintegrate(d)" is understood to mean cut, ground and/or shredded.
The disintegrated plant material may be shredded. In a further example, the disintegrated plant material may be finely disintegrated, i.e. it has an average particle size of less than 2 mm. The particles of the finely disintegrated plant material, such as finely disintegrated tobacco material, may be sized to pass through a screen of about 10 (US) mesh, i.e. sieve size 2.0 mm, or 18 (US) mesh, i.e. sieve size 1 .0 mm.
In this document, the term "snuff' used in the context of oral smokeless moist snuff composition and/or oral smokeless moist snuff product may intend fermented snuff and/or pasteurized snuff. Thus, the snuff may be American-type moist snuff and/or
Scandinavian-type moist snuff (i.e. snus). An oral smokeless moist tobacco composition is an oral smokeless moist snuff composition wherein the disintegrated plant material comprises or consists of tobacco. Addition of particles containing a flavorant as described herein to the oral smokeless moist tobacco composition provides an oral smokeless moist tobacco product. The tobacco may be mixed with non-tobacco fibres as decribed herein.
An oral smokeless moist non-tobacco composition is an oral smokeless moist snuff composition wherein the disintegrated plant material comprises or consists of non-tobacco fibres. Addition of particles containing a flavorant as described herein to the oral smokeless moist non-tobacco composition provides an oral smokeless non-tobacco product. As an example, the oral smokeless moist non-tobacco composition and/or the oral smokeless non-tobacco product does not comprise tobacco material such as disintegrated tobacco.
The tobacco may be any part, e.g. leaves or stems, of any member of the genus
Nicotiana. The tobacco may be whole or disintegrated, i.e. shredded, cut, ground, cured. Further, the tobacco may be aged, fermented or treated otherwise. The tobacco may include types of material such as flue-cured tobacco, burley tobacco, oriental tobacco, Maryland tobacco, dark tobacco, dark-fired tobacco, dark air cured or light air cured and Rustica tobaccos as well as other rare or specialty tobaccos. The tobacco of the present disclosure may contain a single type of tobacco or different types of tobacco. The tobacco can have the form of processed tobacco parts or pieces, cured and aged tobacco in substantially natural lamina or stem form, a tobacco extract, extracted tobacco pulp or a mixture of the foregoing. The tobacco may be mixed together with non-tobacco fibres. The tobacco contains salt such as sodium chloride and/or potassium chloride. The total chloride content, i.e. the chloride originating from chloride salts such as sodium and potassium chloride, may be within the range of from about 3 to about 8 % by weight such as from about 3 to about 6 % by weight based on the weight of the tobacco flour, said tobacco flour may contain about 7 % by weight of water. The chloride content of the disintegrated tobacco or the disintegrated non-tobacco plant material may be about 3 % by weight or about 4 % by weight based on the weight of the tobacco flour, said tobacco flour may contain about 7 % by weight of water. The non-tobacco plant fibres may be fibres from non-tobacco plants such as maize fibers, oat fibers, tomato fibers, barley fibers, rye fibers, sugar beet fibers, buck wheat fibers, potato fibers, cellulose fibers, apple fibers, cocoa fibers, bamboo fibers and citrus fibers. The non-tobacco plant fibres may be whole or disintegrated, i.e. shredded, cut, ground. Further, the non-tobacco plant fibres may be cured, aged, fermented or treated otherwise. The amount of non-tobacco plant fibers, such as bamboo fibers, in the smokeless tobacco composition may be within the range of from about 1 to about 60% w/w or from about 2 to about 20% w/w based on dry weight of the smokeless tobacco composition. Micro Crystalline Cellulose may also be used as an alternative.
The non-tobacco fibers may have an average length-to-width ratio equal to or greater than 3.5:1 and equal to or lower than 100:1 . The non-tobacco plant fibers may originate from bamboo. The non-tobacco fibers may have an average length-to-width ratio equal to or lower than 25:1 . The non-tobacco fibers may have an average length-to-width ratio equal to or greater than 6:1. The non-tobacco fibers may have an average length-to-width ratio equal to or greater than 10:1 . The non-tobacco fibers may have an average length- to- width ratio equal to or greater than 15:1.
The oral smokeless moist snuff product described herein may be provided in particulate form, as a loose powder, or be portion-packaged in a pouch. The pouch may be made of a water-permeable material so that extraction of components such as nicotine and/or flavorant may easily take place when the product is placed in a user's mouth.
The encapsulation of the flavorant in the microcapsule or granule may be encapsulation of the flavorant by a shell such as a coating. Alternatively or additionally, the flavorant encapsulation may be that the flavorant is contained in a matrix. For instance, the flavorant may be dispersed within a matrix. The matrix may be enclosed by a shell or coating. The shell and/or the matrix may comprise or consist of a cellulose-derivatized polymer selected from the group consisting of hydroxypropyl methylcellulose,
hydroxypropyl cellulose, methyl cellulose and any combinations thereof. As an example, there is provided an oral smokeless moist snuff product as described herein, wherein the flavorant is encapsulated by a coating comprising a cellulose-derivatized polymer as described herein. The cellulose-derivatized polymer may be hydroxypropyl
methylcellulose. The cellulose-derivatized polymer described herein may be mixed with further ingredients. For instance, the cellulose-derivatized polymer may be mixed with talcum powder. As an example, hydroxypropylmethyl cellulose may be mixed with talcum powder. In a further example, the microcapsule or granule flavorant of the oral smokeless moist snuff product described herein is encapsulated by an inner coating and an outer coating. The inner coating may comprise or consist of gelatine. The outer coating may comprise or consist of a cellulose-derivatized polymer selected from the group consisting of hydroxypropyl methylcellulose, hydroxypropyl cellulose, methyl cellulose and any combinations thereof. As an example, the outer coating may comprise or consist of hydroxypropyl methylcellulose. In a further example, the inner coating comprises or consists of gelatine, and the outer coating comprises or consists of hydroxypropyl methylcellulose optionally in combination with talcum powder. The outer coating is salt-sensitive so that it substantially remains in a solid state in the presence of a salt selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate and potassium lactate and any combinations thereof in the amounts indicated herein. When the salt concentration is lowered, such as upon saliva excretion in a user's mouth, the outer coating softens and/or dissolves so that the gelatine inner coating is exposed. Since gelatine will soften and/or dissolve upon contact with the moisture present in the oral smokeless moist snuff product the flavorant will be released. In order to prevent or minimize flavorant release during storage and prior to being placed in a user's mouth, the outer coating should cover most of the inner coating. Advantageously, the outer coating should be free or substantially free from cracks.
The oral smokeless moist snuff product described herein comprises one or more salts selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combinations thereof. The sodium chloride may be replaced entirely or partly with potassium chloride.
It will be appreciated that when the one or more salts is a combination of different salts each salts may be present in an amount sufficient to contribute to cellulose-derivatized polymer cloud point lowering in the oral smokeless moist snuff product. As an example, the one or more salts of the oral smokeless moist snuff product described herein may comprise or consist of sodium chloride, sodium carbonate and potassium sulphate. In a further example, the one or more salts of the oral smokeless moist snuff product described herein may comprise or consist of sodium sulphate and/or potassium sulphate and one or more salts selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate and any combination thereof. In still a further example, the one or more salts of the oral smokeless moist snuff product described herein comprises sodium carbonate, sodium chloride and optionally one or more salts selected from the group consisting of potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combination thereof. Further, the sodium chloride may be replaced entirely or partly with sodium sulphate or potassium sulphate. Replacing the sodium chloride with sodium sulphate and/or potassium sulphate may affect the flavour profile of the product, which may be desirable to meet the demands of certain users. Unexpectedly, the inventors of the present disclosure have found that sodium chloride may be exchanged for sodium sulphate and/or potassium sulphate to at least some extent without affecting the cloud point of the cellulose-derivatized polymer of the particles containing a flavorant.
The one or more salts may be mixed with the disintegrated plant material such as tobacco or with the non-tobacco plant fibres. Additionally, the one or more salts may be contained in the microcapsules. As an example, the one or more salts may be contained in the microcapsule or granule shell or the microcapsule or granule matrix. In a further example, the one or more salts is mixed with the disintegrated plant material such as tobacco or non-tobacco plant fibres and also contained in the microcapsules or granules. As described herein, the one or more salts selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combinations thereof are believed to have a so-called salting in effect whereby the integrity of the particles containing a flavorant such as microcapsules or granules is maintained until the salt concentration is lowered.
Further, it will be appreciated that the one or more salts of the oral smokeless moist snuff composition and/or the oral smokeless moist snuff product includes the sodium chloride and/or the potassium chloride occurring naturally in the disintegrated plant material. Thus, the one or more salts of the oral smokeless moist snuff composition and/or the oral smokeless moist snuff product includes added salts as well as sodium chloride and/or potassium chloride occurring naturally in the disintegrated plant material.
It will be appreciated that the one or more salts described herein includes salts commonly used in snuff, such as sodium chloride, as well as salts used as pH adjusters, such as sodium carbonate. Sodium chloride provides a salty taste and/or antimicrobial activity and may also influence the cellulose-derivatized polymer cloud point. Sodium carbonate provides pH adjustment and may also influence the cellulose-derivatized polymer cloud point. Thus, in addition to lowering the cloud point of the cellulose-derivatized polymer the one or more salts may provide taste, pH adjustment, antimicrobial activity etc. The one or more salts may be sodium lactate and/or potassium lactate. This may be advantageous since sodium lactate and/or potassium lactate have a neutral taste, an antibacterial activity and are also believed to have a lower impact on a cellulose- derivatized polymer than, for instance, sodium chloride. As an example, all or at least part of the sodium chloride may be exchanged for sodium lactate and/or potassium lactate.
In a further example, the one or more salts may be selected from the group consisting of sodium chloride, potassium carbonate, potassium sulphate and any combinations thereof. In a further example, the one or more salts may comprise sodium carbonate and a salt selected from the group consisting of potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combination thereof.
In still a further example, the one or more salts may comprise potassium carbonate and a salt selected from the group consisting of sodium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combination thereof.
Further, the one or more salts of the oral smokeless moist snuff product described herein may comprise or consist of sodium chloride, sodium carbonate and potassium sulphate. The ratio sodium chloride: sodium carbonate: potassium sulphate may be about 6:3:1 or about 7:2:1 . It will be appreciated that the potassium sulphate may be replaced entirely or partly with sodium chloride and/or potassium chloride. Thus, the one or more salts of the oral smokeless moist snuff product described herein may comprise or consist of sodium carbonate and sodium chloride and/or potassium chloride.
Further, the one or more salts of the oral smokeless moist snuff product described herein may comprise or consist of sodium chloride, sodium carbonate and optionally one or more salts selected from the group consisting of potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combinations thereof.
The one or more salts of the oral smokeless moist snuff product described herein may comprise or consist of sodium sulphate and/or potassium sulphate and/or one or more salts selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate and any combinations thereof.
The total amount of the one or more salts of the oral smokeless moist snuff composition and/or the oral smokeless moist snuff product prepared for the consumer may be estimated using any method known in the art to a skilled person. For instance, the total amount of the one or more salts may be estimated or indicated based on the
measurement of ionic strength or conductivity. The amount of the one or more salts will depend on the total amount of moisture of the oral smokeless moist snuff composition. Generally, to maintain flavorant particle integrity in the oral smokeless moist snuff product the amount of the one or more salts will have to be increased when the total amount of moisture of the oral smokeless moist snuff composition is raised. The inventors of the present disclosure have found that for a total amount of moisture within the range of from about 35% by weight to about 60% by weight based on the total weight of the oral smokeless moist snuff composition, the total amount of the one or more salts should be within the range of about 15 % by weight to about 35 % by weight based on the total weight of water and total weight of the one or more salts in the oral smokeless moist snuff composition. The amount of particles containing a flavorant as described herein may be within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product. For instance, the amount of particles containing a flavorant may be within the range of from about 5 % by weight to about 25 % by weight, from about 5% by weight to about 20 % by weight, from about 5 % by weight to about 15 % by weight, from about 5 % by weight to about 10 % by weight or from about 10 % by weight to about 20 % by weight based on the total weight of the oral smokeless moist snuff product. In a further example, the amount of particles containing a flavorant may be about 5 % by weight, about 10 % by weight, about 15 % by weight or about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
As an example, in the oral smokeless moist snuff composition of the oral smokeless moist snuff product described herein the total amount of the one or more salts may be within the range of from about 15 % by weight to about 35 % by weight, from about 15 % by weight to about 25 % by weight or from about 20 % by weight to about 25 % by weight, based on the total weight of water and the total weight of the one or more salts of the oral smokeless moist snuff composition, and the total amount of moisture may be within the range of from about 45 % by weight to about 60 % by weight based on the total weight of the oral smokeless moist snuff composition. The amount of particles containing a flavorant as described herein may be within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product. For instance, the amount of particles containing a flavorant may be within the range of from about 5 % by weight to about 25 % by weight, from about 5% by weight to about 20 % by weight, from about 5 % by weight to about 15 % by weight, from about 5 % by weight to about 10 % by weight or from about 10 % by weight to about 20 % by weight based on the total weight of the oral smokeless moist snuff product. In a further example, the amount of particles containing a flavorant may be about 5 % by weight, about 10 % by weight, about 15 % by weight or about 20 % by weight based on the total weight of the oral smokeless moist snuff product. In a further example, in the oral smokeless moist snuff composition of the oral smokeless moist snuff product described herein the total amount of the one or more salts may be within the range of from about 15 % by weight to about 35 % by weight, from about 15 % by weight to about 25 % by weight or from about 20 % by weight to about 25 % by weight, based on the total weight of water and the total weight of the one or more salts of the oral smokeless moist snuff composition, and the total amount of moisture may be within the range of about 33 % by weight to about 37 % by weight such as about 35 % by weight based on the total weight of the oral smokeless moist snuff composition. The amount of particles containing a flavorant as described herein may be within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product. For instance, the amount of particles containing a flavorant may be within the range of from about 5 % by weight to about 25 % by weight, from about 5% by weight to about 20 % by weight, from about 5 % by weight to about 15 % by weight, from about 5 % by weight to about 10 % by weight or from about 10 % by weight to about 20 % by weight based on the total weight of the oral smokeless moist snuff product. In a further example, the amount of particles containing a flavorant may be about 5 % by weight, about 10 % by weight, about 15 % by weight or about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
In a further example, in the oral smokeless moist snuff composition of the oral smokeless moist snuff product described herein the total amount of the one or more salts may be within the range of from about 15 % by weight to about 35 % by weight, from about 15 % by weight to about 25 % by weight or from about 20 % by weight to about 25 % by weight, based on the total weight of water and the total weight of the one or more salts of the oral smokeless moist snuff composition, and the total amount of moisture may be within the range of about 38 % by weight to about 42 % by weight such as about 40 % by weight based on the total weight of the oral smokeless moist snuff composition. The amount of particles containing a flavorant as described herein may be within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product. For instance, the amount of particles containing a flavorant may be within the range of from about 5 % by weight to about 25 % by weight, from about 5% by weight to about 20 % by weight, from about 5 % by weight to about 15 % by weight, from about 5 % by weight to about 10 % by weight or from about 10 % by weight to about 20 % by weight based on the total weight of the oral smokeless moist snuff product. In a further example, the amount of particles containing a flavorant may be about 5 % by weight, about 10 % by weight, about 15 % by weight or about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
In a further example, in the oral smokeless moist snuff composition of the oral smokeless moist snuff product described herein the total amount of the one or more salts may be within the range of from about 15 % by weight to about 35 % by weight, from about 15 % by weight to about 25 % by weight or from about 20 % by weight to about 25 % by weight, based on the total weight of water and the total weight of the one or more salts of the oral smokeless moist snuff composition, and the total amount of moisture may be within the range of about 43% by weight to about 47 % by weight such as about 45 % by weight based on the total weight of the oral smokeless moist snuff composition. The amount of particles containing a flavorant as described herein may be within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product. For instance, the amount of particles containing a flavorant may be within the range of from about 5 % by weight to about 25 % by weight, from about 5% by weight to about 20 % by weight, from about 5 % by weight to about 15 % by weight, from about 5 % by weight to about 10 % by weight or from about 10 % by weight to about 20 % by weight based on the total weight of the oral smokeless moist snuff product. In a further example, the amount of particles containing a flavorant may be about 5 % by weight, about 10 % by weight, about 15 % by weight or about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
In a further example, in the oral smokeless moist snuff composition of the oral smokeless moist snuff product described herein the total amount of the one or more salts may be within the range of from about 15 % by weight to about 35 % by weight, from about 15 % by weight to about 25 % by weight or from about 20 % by weight to about 25 % by weight, based on the total weight of water and the total weight of the one or more salts of the oral smokeless moist snuff composition, and the total amount of moisture may be within the range of about 48 % by weight to about 52 % by weight such as about 50 % by weight based on the total weight of the oral smokeless moist snuff composition. The amount of particles containing a flavorant as described herein may be within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product. For instance, the amount of particles containing a flavorant may be within the range of from about 5 % by weight to about 25 % by weight, from about 5% by weight to about 20 % by weight, from about 5 % by weight to about 15 % by weight, from about 5 % by weight to about 10 % by weight or from about 10 % by weight to about 20 % by weight based on the total weight of the oral smokeless moist snuff product. In a further example, the amount of particles containing a flavorant may be about 5 % by weight, about 10 % by weight, about 15 % by weight or about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
In a further example, in the oral smokeless moist snuff composition of the oral smokeless moist snuff product described herein the total amount of the one or more salts may be within the range of from about 15 % by weight to about 35 % by weight, from about 15 % by weight to about 25 % by weight or from about 20 % by weight to about 25 % by weight, based on the total weight of water and the total weight of the one or more salts of the oral smokeless moist snuff composition, and the total amount of moisture may be within the range of about 53 % by weight to about 57 % by weight such as about 55 % by weight based on the total weight of the oral smokeless moist snuff composition. The amount of particles containing a flavorant as described herein may be within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product. For instance, the amount of particles containing a flavorant may be within the range of from about 5 % by weight to about 25 % by weight, from about 5% by weight to about 20 % by weight, from about 5 % by weight to about 15 % by weight, from about 5 % by weight to about 10 % by weight or from about 10 % by weight to about 20 % by weight based on the total weight of the oral smokeless moist snuff product. In a further example, the amount of particles containing a flavorant may be about 5 % by weight, about 10 % by weight, about 15 % by weight or about 20 % by weight based on the total weight of the oral smokeless moist snuff product. In a further example, in the oral smokeless moist snuff composition of the oral smokeless moist snuff product described herein the total amount of the one or more salts may be within the range of from about 15 % by weight to about 35 % by weight, from about 15 % by weight to about 25 % by weight or from about 20 % by weight to about 25 % by weight, based on the total weight of water and the total weight of the one or more salts of the oral smokeless moist snuff composition, and the total amount of moisture may be within the range of about 58 % by weight to about 62 % by weight such as about 60 % by weight based on the total weight of the oral smokeless moist snuff composition. The amount of particles containing a flavorant as described herein may be within the range of from about 1 % by weight to about 25 % by weight based on the total weight of the oral smokeless moist snuff product. For instance, the amount of particles containing a flavorant may be within the range of from about 5 % by weight to about 25 % by weight, from about 5% by weight to about 20 % by weight, from about 5 % by weight to about 15 % by weight, from about 5 % by weight to about 10 % by weight or from about 10 % by weight to about 20 % by weight based on the total weight of the oral smokeless moist snuff product. In a further example, the amount of particles containing a flavorant may be about 5 % by weight, about 10 % by weight, about 15 % by weight or about 20 % by weight based on the total weight of the oral smokeless moist snuff product.
In a further example, there is provided an oral smokeless moist snuff product comprising: (a) an oral smokeless moist snuff composition comprising:
- disintegrated plant material,
- sodium chloride, sodium carbonate and optionally potassium sulphate, and
- water,
wherein the total amount of the one or more salts is about 25 % by weight based on the total weight of water and total weight of the one or more salts in the oral moist smokeless snuff composition,
wherein the total amount of moisture is about 46 % by weight based on the total weight of the oral smokeless moist snuff composition;
(b) particles comprising a flavorant and hydroxypropyl methylcellulose,
wherein the amount of said particles is about 10 % by weight based on the total weight of the oral smokeless moist snuff product. Additionally, the oral smokeless moist snuff product may comprise from about 1 to about 5 % by weight, such as from about 2 to about 4 % by weight, based on the dry weight of the oral smokeless moist snuff composition, of a humectant selected from the group consisting of propylene glycol and glycerol. The oral smokeless moist snuff product described herein may comprise no or substantially no humectant. It will be appreciated that the humectant should be selected in such a way and/or in an amount that it influences the cloud point of the cellulose-derivatized polymer to only a small extent or not at all. For instance, glycerol will have only a small impact on the cellulose polymer cloud point whereas propylene glycol will have a larger impact. Therefore, in case propylene glycol is used the amount should be adjusted to avoid a too large impact on the cellulose cloud point. For instance, propylene glycol in an amount of about 2 to about 4 % by weight, such as from about 0.5 to about 2 % by weight, such as from about 1 to about 3 % by weight, such as from about 1 to about 2 % by weight, based on the dry weight of the oral smokeless moist snuff composition, may be added to the oral smokeless moist snuff product described herein. The impact of the humectant on the cellulose-derivatized polymer cloud point may at least to some extent be compensated for by increasing the amount of the one or more salts. The humectant of the oral smokeless moist snuff product described herein may contain a humectant comprising or consisting of glycerol.
As used herein, the term "total amount of moisture" refers to the total amount of oven volatile ingredients, such as water and other oven volatiles (e.g. propylene glycol, ethanol etc.) in the preparation, composition or product referred to. The total amount of moisture is given herein as percent by weight (wt%) of the total weight of the preparation, composition or product referred to. The total amount of moisture as referred to herein may be determined by using the LOD method disclosed in the Examples in which the oven volatile content at a temperature of about 105°C is determined. Thus, the total amount of moisture may refer to the total amount of oven volatiles measured of a temperature at about 105°C, such as measured with an LOD method. In this document, the expressions "total amount of moisture", "moisture content" and "moisture level" are used interchangeably. The total amount of moisture of the oral smokeless moist snuff composition may range from about 35 % by weight to about 60 % by weight such as from about 40 % by weight to about 60 % by weight, from about 45 % by weight to about 60 % by weight, from about 45 % by weight to about 55 % by weight, from about 50 % by weight to about 55 % by weight, from about 50 % by weight to about 60 % by weight or from about 55 % by weight to about 60 % by weight. For instance, the total amount of moisture of the oral smokeless moist snuff composition may be about 35 % by weight, about 40% by weight, about 45 % by weight, about 46 % by weight, about 55 % by weight or about 60 % by weight.
The water content of the oral smokeless moist snuff composition and/or the oral smokeless moist snuff product includes all water present such as added water and water occurring naturally in the disintegrated plant material.
In accordance with the present disclosure, there is provided an oral smokeless moist snuff product as described herein wherein the total amount of moisture of the oral smokeless moist snuff composition is about 40 % by weight. The one or more salts comprises or consists of sodium chloride, sodium carbonate and potassium sulphate. The ratio sodium chloride: sodium carbonate: potassium sulphate may be about 6:3:1 or about 7:2:1.
In accordance with the present disclosure, there is provided an oral smokeless moist snuff product as described herein wherein the total amount of moisture of the oral smokeless moist snuff composition is about 46 % by weight, and the one or more salts may comprise or consist of sodium chloride, sodium carbonate and potassium sulphate. The ratio sodium chloride: sodium carbonate: potassium sulphate may be about 7:2:1. In accordance with the present disclosure, there is provided an oral smokeless moist snuff product as described herein wherein the total amount of moisture of the oral smokeless moist snuff composition is about 55 % by weight, and the one or more salts may comprise or consist of sodium chloride, sodium carbonate and potassium sulphate. The ratio sodium chloride: sodium carbonate: potassium sulphate may be about 7:2:1.
In accordance with the present disclosure, there is provided an oral smokeless moist snuff product as described herein wherein the total amount of moisture is about 35 wt%, and the one or more salts may comprise or consist of sodium chloride and sodium carbonate. The ratio sodium chloride: sodium carbonate may be about 3:1.
In accordance with the present disclosure, there is provided an oral smokeless moist snuff product as described herein wherein the total amount of moisture of the oral smokeless moist snuff composition is about 46 wt%, and the one or more salts may comprise or consist of sodium chloride and sodium carbonate. The ratio sodium chloride: sodium carbonate may be about 3:1 or about 4:1 .
In accordance with the present disclosure, there is provided an oral smokeless moist snuff product as described herein wherein the total amount of moisture is about 55 wt% of the oral smokeless moist snuff composition, and the one or more salts may comprise or consist of sodium chloride and sodium carbonate. The ratio sodium chloride: sodium carbonate may be about 4:1.
The particles described herein may be microparticles, such as microcapsules or granules as described herein. The particles may or may not contain a carrier.
The particles such as microcapsules or granules of the present disclosure contain a flavorant. As used herein, the terms "flavorant", "flavor" "flavoring agent" or the like denote a substance used to influence the aroma and/or taste of the oral smokeless moist snuff product.
In this document, whenever the particles are described with respect to microcapsules it will be appreciated that the term microcapsules may be exchanged for granules, capsules, microparticles etc. The flavorant may be a single flavor or a combination of flavorants/flavors. The flavorant may be in solid or liquid form. The liquid form may be a liquid composition such an oil. For instance, the flavorant may be an essential oil, a compounded flavoring and/or extracts. Further, the flavorant may be natural or synthetic. Examples of flavorants include menthol, peppermint, spearmint, liquorice, anethol, geranium, lemon oil, orange oil, grapefruit oil, bergamot oil, vanilla, coffee, coconut, almond, pecan, walnut, peanut, hazelnut, ginger, fennel, clove, anise, cardamom, coriander, basil, oregano, rosemary, thyme, sage, jasmine, lavender, wintergreen, cocoa and cumarin. Further, the flavor may contain tobacco flavorant. Alternatively, the flavorant may be a non-tobacco flavorant.
As an example, the flavorant may be a solid encapsulated by a shell such as a coating comprising, for instance, hydroxypropyl methylcellulose, to provide a granule or microcapsule. In a further example, the flavorant may be dispersed within a matrix and optionally encapsulated by a shell such as a coating comprising, for instance,
hydroxypropyl methylcellulose, to provide a granule or microcapsule.
The particles containing a flavorant such as microcapsules may be a mixture of microcapsules containing different flavorants. For instance, 50% of the microcapsules may contain a first flavorant and the remaining 50% may contain a second flavorant different from the first flavorant.
When the particles contain an inner coating and/or an outer coating, then the inner coating and/or the outer coating of the microcapsules may or may not contain a flavor. As an example, the inner and/or the outer coating contain no flavor. In a further example, the inner and/or outer contain a non-tobacco flavor.
The total weight of the particles containing a flavorant such as microcapsules contained within the oral smokeless moist snuff product may vary. For instance, the amount of said particles may be within the range of from about 1 % by weight to about 25 % by weight , such as from about 5 % by weight to about 25 % by weight or from about 5 % by weight to about 10 % by weight, based on the total weight of the oral smokeless moist snuff product. As an example, the amount of said particles may be about 5 % by weight, about 10 % by weight, about 15 % by weight or about 20 % by weight. In a further example, the amount of said particles may be about 10 % by weight. The particles , such as microcapsules or granules, containing a flavorant may be mixed with an oral smokeless moist snuff composition to provide the oral smokeless moist snuff product. For instance, the particles containing a flavorant may be added to the oral smokeless moist snuff composition or vice versa. Alternatively, the particles containing a flavorant and the components of the oral smokeless moist snuff composition may be mixed in any order to provide the oral smokeless moist snuff product. If desired, a single particle such as a capsule or granule having a size larger than that of the microcapsules or granules may be used in addition to or instead of a plurality of microcapsules and/or granules. The single capsule may contain a flavorant that is the same as or different from that of the microcapsules and/or granules.
The shape of the particles, such as microcapsules or granules, may vary, but typically the microcapsules or granules have a substantially spherical shape. Alternatively, the microcapsules or granules may have other types of shapes such as rectilinear, oblong, elliptical or oval shapes.
The particles containing a flavorant such as microcapsules or granules may be uniform or varied in size. The microcapsule or granule diameter may be from 1 to 5 mm, such as from 1 to 4 mm or from 1 to 3 mm or from 300 micrometers to 1 mm. Further, the microcapsules or granules may be spherical and have a diameter equal to or less than about 300 micrometers, such as from 100-300 micrometers, such as from 100-200 micrometers, or from 1 to 40 micrometers or from 1 to 20 micrometers. As an example, the microcapsule or granule diameter may be about 1 mm. In some oral smokeless moist snuff products it may be desired to include microcapsules or granules of substantially uniform size, whereas in other oral smokeless moist snuff products it may be desired to include microcapsules or granules with varying size.
If desired, particles such as microcapsules of different sizes and types may be included in the oral smokeless moist snuff products to provide for a desired flavor release profile. For example, a first flavorant may be released from a first set of microcapsules or granules, and a second flavorant may be released from a second set of microcapsules or granules. The release of the first flavorant may take place prior to, at the same time as or after release of the second flavorant. The particles containing a flavorant described herein may be dyed. The dye may be provided by a color additive approved for use in food. By providing at least part of the particles as dyed particles the consumer may perceive the oral smokeless moist snuff product as more interesting and/or appealing.
The crush strength of the microcapsules disclosed herein is sufficient to allow for normal handling and storage without significant premature or undesirable breakage.
If desired, a non-encapsulated flavorant may be mixed with the disintegrated plant material such as tobacco or non-tobacco plant fibres of the oral smokeless moist snuff product described herein. For instance, the flavorant may be added by spraying it onto the tobacco or the non-tobacco plant fibres. The flavorant may be sprayed directly onto loose tobacco and/or non-tobacco fibres or onto pouches containing tobacco and/or non- tobacco fibres. In this way, a user placing the oral smokeless moist snuff product described herein into his or her mouth will immediately experience the flavorant mixed with the tobacco or non-tobacco plant fibres and then gradually also experience the flavorant released from the microcapsules. The non-encapsulated flavorant may be the same or different from that contained in the particles containing a flavorant such as microcapsules or granules. In this way, a consumer may perceive the taste of the oral smokeless moist snuff product to evolve and/or change over time.
Alternatively or additionally, a non-encapsulated flavorant may be added to the oral smokeless moist snuff product described herein by coating at least part of one inside surface, such as an inside lid or bottom surface, of a container with the flavorant, adding the oral smokeless moist snuff product to the container and closing of the container. The container may be a packaging container for an oral smokeless moist snuff product. When the container is closed, the flavorant applied to the at least part of one inside surface of the container will flavorize the oral smokeless moist snuff product. Accordingly, there is provided a method for adding a flavorant to an oral smokeless moist snuff product as described herein, said method comprising the steps of:
a) applying a flavorant onto at least part of one inside surface of a container for an oral smokeless moist snuff product,
b) placing the oral smokeless moist snuff product as described herein in the container, and
c) closing the container. It will be appreciated that the container for an oral smokeless moist snuff product does not form part of the oral smokeless moist snuff product described herein. Depending on the flavorant used in the tobacco and/or non-tobacco plant material and the flavorant of the particles such as microcapsules or granules the overall result for a user may be a constant flavor intensity, an increase in flavor intensity over a certain time, a change in flavour etc. The oral smokeless moist snuff product may further comprise a sweetener. Suitable sweeteners include natural sweeteners such as fructose, sucrose, glucose, maltose, mannose, galactose, lactose or xylitol. The sweetener may also be an artificial sweetener such as sucralose, saccharin, aspartame, acesulfame K, neotam or stevia. The sweetener may be mixed with the oral smokelss moist snuff composition and/or be provided in encapsulated form.
A pH adjusting agent may be included in the oral smokeless moist snuff product described herein to provide a desired pH value. The pH adjusting agent may be an alkali metal base or an acid. The alkali metal base may be sodium hydroxide or potassium hydroxide. The acid may be acetic acid, lactic acid or citric acid. The pH adjusting agent may be mixed with the oral smokelss moist snuff composition and/or be provided in encapsulated form.
A buffering agent may be present in the oral smokeless moist snuff product described herein in order to maintain pH close to a desired value. Suitable buffering agents include alkali metal carbonates and alkali metal bicarbonates. The alkali metal carbonates may be sodium carbonate or potassium carbonate. The alkali metal bicarbonates may be sodium bicarbonate or potassium bicarbonate. The buffering agent may be mixed with the oral smokelss moist snuff composition and/or be present in encapsulated form. The oral smokeless moist snuff described herein may also include additives such as disintegration aids, antioxidants, binders, colorants, fillers, thickening agents and/or combinations thereof. The additives may be mixed with the oral smokelss moist snuff composition and/or be present in encapsulated form or in non-encapsulated form. The particles described herein such as microcapsules or granules may be manufactured by coating a gelatine microcapsule with a cellulose polymer such as hydroxypropyl methylcellulose using fluidized bed technique. However, any other technique known in the art to the skilled person may be used. The oral smokeless moist snuff product described herein may be manufactured by dispersing the microcapsules with the other components of the oral smokeless moist snuff.
Further aspect
In a further aspect, there is provided an oral smokeless moist snuff product comprising: a) from 14 to 66 wt% of disintegrated plant material, b) from 0.5 to 20 wt% of microcapsules comprising a flavorant encapsulated by a cellulose polymer selected from the group consisting hydroxypropyl methylcellulose, hydroxypropyl cellulose, methyl cellulose and any combination thereof, c) from 1 .5 to 18 wt% of salt selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combination thereof, wherein the moisture content of the product is within the range of from 30 to 60 wt%.
DEFINITIONS
In this document, particulate is used for a particle size of the product which enables the final product to be provided in so-called loose form, from which a pinch of snus may be made in individual sized by a user of a product.
As used herein, the term "user" is used interchangeably with the term "consumer" and the term "human". Further, the expressions "oral" or "oral use" refer to use in the oral cavity, i.e. for chewing purposes or buccal placement.
The term "g" stands for gram or grams. The term "mm" stands for millimeters. LOD stands for Loss On Drying and is a method to measure the loss of weight of the sample when dried at 105°C. The sample is dried until the sample weight is substantially constant. The LOD method is described in the Examples section.
The term "wt%" stands for weight% means weight percent in the composition or product referred to. The terms "wt%", "weight%" and "% by weight" are used interchangeably.
HPMC is an abbreviation for hydroxypropyl methylcellulose.
As used herein, the expressions "particle containing a flavorant" and "flavorant particle" are used interchangeably.
The term rpm stands for revolutions per minute.
The term GC stands for Gas Chromatography. The term MS stands for Mass Spectroscopy. The term GCMS stands for Gas Chromatography Mass Spectroscopy. The term w/w stands for weight by weight.
BRIEF DESCRIPTION OF THE DRAWINGS
Figure 1 shows a graph indicating flavor intensity experienced by eleven test persons during a time period of 60 minutes.
The disclosure is illustrated by the following non-limitative Examples.
EXAMPLES
The following equipment and general procedures were used in the Examples below. General
Headspace screw top vials (20 ml) were purchased from ThermoScientific. Petroleum ether Suprasolv was purchased from VWR. Samples were shaken on an incubation orbital shaker, professional 3500, purchased from VWR. Analyses were performed on an Agilent 5890/5972/7673 GCMS-system, operating in full scan mode. GC column was an Agilent Innowax (60 m x 0.25 mm x 0.25 urn).
Measurements
Snus samples were extracted with two different extraction methods, one for total flavor and one for free flavor. In this document, total flavor intends the total analyzed amount of flavor in the product consisting of moist snus and microcapsules. Thus, the total flavor intends the sum of the flavor of the microcapsules and the flavor contained in the moist snus. In this document, free flavor intends the analyzed amount of flavor in the moist snus. Thus, the free flavor intends the flavor contained in the moist snus, excluding the flavor of the non-disintegrated microcapsules. Unless otherwise indicated, in all
Examples the flavor is a mixture of peppermint and menthol. After extraction a GC/MS method (the same method for both extractions) was used to estimate the amount of flavor in the extracts. This was a semi-quantitative method for menthol, which served as a marker for all flavor compounds. The area of menthol was integrated and area units were compared between samples.
Extraction of total flavor
For each replicate 0.5-1 g of snus or one pouch (cut in two pieces) was put into a headspace vial. 5 ml of tap water was added. The samples were shaken for 5 min at ambient temperature (360 rpm). Thereafter 5 ml of petroleum ether was added before samples were shaken for 60 minutes at 50 °C (360 rpm). After cooling samples were put on GC-vials and analyzed with GC/MS. Extraction of free flavor
For each replicate 0.5-1 g of snus or one pouch (cut in two pieces) was put in to a headspace vial. 5 ml of petroleum ether was added. The samples were shaken for 5 min at ambient temperature (360 rpm). After 5 minutes of sedimentation samples were put on GC-vials and analyzed with GC/MS. The area as measured by GC/MS is indicated in Table 3. Tobacco
In the examples below, grinded and heated moist tobacco refers to tobacco that has been prepared as follows. The tobacco was grinded and pasteurized, and the moisture content was adjusted with water to about 35 wt%. The chloride content of the tobacco flour prior to grinding and pasteurization, i.e. the sum of chloride from NaCI and KCI, was about 3. wt% based on the weight of the tobacco flour. The total amount of moisture of the tobacco flour was 7 wt%. Moist snus versus moist snus product
In the examples below, "moist snus" refers to a mixture of grinded and heated moist tobacco, sodium carbonate, potassium sulphate, sodium chloride, ethanol and water. In some examples the potassium sulphate was excluded. Further, in the examples below "moist snus product" refers to the mixture resulting from adding microcapsules to the moist snus, i.e. a mixture of microcapsules, grinded and heated moist tobacco, sodium carbonate, potassium sulphate, sodium chloride, ethanol and water. In some examples the potassium sulphate was excluded. LOP method
In all the following examples, the moisture content of each of the tobacco material and the non-tobacco plant fibers, if present, was determined by using a method based on literature references Federal Register/ vol.74, no. 4/712-719/Wednesday, January 7, 2009/Notices, "Total moisture determination" and AOAC (Association of Official Analytical Chemics), Official Methods of Analysis 966.02: "Moisture in Tobacco" (1990), Fifth Edition, K. Helrich (ed). In this method, the oven volatile (OV) content of the tobacco material and the non-tobacco plant fibers, if present, is measured as described
hereinafter. The moisture content (i.e. the oven volatile content) of each of the tobacco material and the non-tobacco plant fibers, if present, was determined gravimetrically by taking 2.5±0.25 g sample and weighing the sample before evaporation of moisture and after evaporation of moisture. Mettler Toledo's Moisture Analyzer HB43, a balance with halogen heating technology, was used (instead of an oven and a balance as in the mentioned literature references). The sample was heated to 105 °C (instead of 99.5±0.5 °C as in the mentioned literature references). The measurement was stopped when the weight change was less than 1 mg during a 90 seconds time period. The moisture content (i.e. oven volatile content) as weight percent of the original weight of the sample is then calculated automatically by the Moisture Analyzer HB43.
As mentioned herein above, the content of oven volatiles other than water (i.e. nonaqueous oven volatiles) in tobacco flour, is normally less than 1 % by weight. Therefore the moisture content of tobacco material as measured using the herein described method substantially corresponds to the actual water content of the tobacco material. In the examples, the given water content of the initial tobacco preparations is the calculated sum of oven volatiles content of the tobacco material and the non-tobacco plant fibers if present, as measured by the above disclosed method, and, where applicable, the amount of water added to the tobacco material in the process.
EXAMPLE 1
Microcapsules were formed in the following manner.
40,0 g of hydroxypropyl methylcellulose, type 2910, viscosity 3 mPa*s (SheffCel 60HD3, purchased from Kerry ) was dissolved in 360 g of purified water resulting in a 400 g weight solution.
For the coating process a fluid bed Mini-Glatt (from Glatt GmbH, Binzen) with bottom spray coating (Wurster) was used. The spray nozzle was 0.5 mm in diameter. The bottom filter was 100 μηη, mounted on a bottom plate with diameter 7.5 cm.
90 g of Millicaps 1000 E_1413279 (from V. MANE FILS, France) was charged in the fluid bed. The Millicaps were substantially gelatin microcapsules containing a liquid
peppermint/menthol flavorant. 230 g of the above prepared solution was sprayed on to the Millicaps 1000 E_1413279. Settings for the process were as indicated in Table 1.
Table 1
Airflow (Nm3/h) 30
Inlet temperature (C°) 50
Product temperature vessel 38-40
(C°)
Spray rate (g/min) 1 .0
Spray pressure (Bar) 1 .4 The formed microcapsules were then sieved through a sieve with a mesh size of 2 mm and the upper fraction was removed.
The moist snus was prepared by mixing sodium carbonate, potassium sulphate, sodium chloride, ethanol and water with grinded and heated moist tobacco. The amounts were as indicated in Table 2 below. Thus, the moist snus of the moist snus product consisted of grinded and heated moist tobacco prepared as described above, sodium carbonate, potassium sulphate, sodium chloride, ethanol and water in amounts as indicated in Table 2.
The above manufactured microcapsules were mixed with the moist snus, said moist snus having a total amount of moisture of about 46 % by weight based on the moist snus, to provide a moist snus product. The composition of the moist snus product is indicated in Table 2.
The moist snus product was packaged in pouches, each pouch having with a weight of about 0.8 g. The pouches were stored in a sealed plastic bag for two weeks at room temperature.
Table 2
After storage for two weeks at room temperature the pouches consisting of moist sn and microcapsules were evaluated regarding chemical storage stability as follows. Table 3
*The free flavor content in Table 3 was calculated as: Free flavor (%) = Average area free flavor / Average area total flavor
Analysis regarding content of menthol was performed in two batches, one for free flavor and one for total flavor. As indicated in Table 3, the free flavor content of the moist snuff was only 4.6% after storage 2 weeks in room temperature. It can be concluded that the HPMC coated gelatin microcapsules containing the liquid flavorant did not release the flavorant to any significant extent. Thus, the HPMC coated gelatin microcapsules containing the liquid flavorant are substantially storage stable in the moist snus.
EXAMPLE 2
Pouches consisting of the moist snus and microcapsules, said pouches being
manufactured as in Example 1 , were evaluated regarding flavor release function as follows. The pouches were stored for two weeks in a sealed plastic bag prior to use.
1 1 test persons used the pouches for 60 minutes. The pouch was put between the gum and the upper lip and the pouch was fixed in that position during the whole test period. After 60 minutes of use, the total amount of menthol left in the used pouches were analyzed and compared to the total amount of analyzed menthol in unused pouches. The test persons used two pouches each. The pouches were analyzed using GC/MS according to the method described above. The results are indicated in Table 4 (Total flavor of unused pouches) and Table 5 (Total flavor of used pouches). The microcapsule flavorant was peppermint and menthol. The analysis was performed with respect to menthol.
Table 4. Unused pouches.
Pouch Total
number Flavor
Area
1 1 105014
2 858570
3 1 154509
4 1221487
5 1017850
6 666178
7 623384
8 475759
9 899776
10 788656
Average
area: 881 1 18.3
Table 5. Used pouches.
The amount of extracted menthol (%) was then calculated as:
Extracted menthol (%) = (Average area unused pouches - Average area used pouches) / (Average area unused pouches). As indicated above, the average area unused pouches is 881 1 18.3, and the average area used pouches is 809610.5. It follows that (881 1 18.3 - 809610.5) / (881 1 18.3) = 8.1 %. Thus, release of menthol from the HPMC coated gelatin microcapsules took place when the test persons used the pouches as indicated above. The test persons were also asked to evaluate their experience of flavorization. The flavor intensity was measured on a scale from 0 to 5, where 0 indicates no experience of flavor and 5 a high experience of flavor intensity. The sensory evaluation was made five and 60 minutes after having placed the oral moist snuff product in the mouth. The mean flavor intensity was calculated for the 1 1 test persons at 5 and 60 minutes respectively, and the result is shown in Figure 1. be concluded that the experienced flavor intensity increased over time.
EXAMPLE 3
Millicaps 1000 E_1413279 were purchased from V. MANE FILS, France. The Millicaps were substantially gelatin microcapsules containing a liquid menthol flavorant.
Moist snus was prepared by mixing sodium carbonate, potassium sulphate, sodium chloride, ethanol and water with grinded and heated moist tobacco. The amounts were as indicated in Table 6 below. Thus, the moist snus of the moist snus product consisted of grinded and heated moist tobacco, sodium carbonate, potassium sulphate, sodium chloride, ethanol and water in amounts as indicated in Table 6.
The Millicaps were mixed with the moist snus, said moist snus having a total amount of moisture of about 46 % by weight based on said moist snus, to provide a moist snus product. The composition of the moist snus product was as indicated in Table 6.
The moist snus product was packaged in pouches, each pouch having a weight of about 0.8 g. 10 pouches were prepared. The pouches were stored for two weeks at room temperature in a sealed plastic bag.
Table 6
After storage for two weeks at room temperature the pouches consisting of moist snus and Millicaps 1000 E_1413279 were analyzed regarding content of menthol according to the GC/MS method described in Example 1. One batch was for free flavor and one was batch for total flavor. As indicated in Table 7, 83 % of the total amount of menthol was found in the moist snus after storage 2 weeks in room temperature. Table 7
Sample Total flavor Sample Free flavor
Number (area) Number (area)
1 668923 1 1 693849
2 656006 12 576435
3 783536 13 598902
4 781676 14 642069
5 774948 15 714342
6 749421 16 496699
7 637317 17 626955
8 788075 18 588688
9 702484 19 625506
10 766540 20 498865
Average 730893 606231
area:
Average 83*
free flavor
(%): *Calculated as: Free flavor (%) = Average area free flavor / Average area total flavor. As indicated above, the average area free flavor is 606231 , and the average area total flavor is 730893. It follows that the free flavor is 606231/ 730893=83%. It can be concluded that the gelatin microcapsules released the menthol flavorant during storage. Thus, the gelatin microcapsules do not exhibit storage stability in the moist snus. Further, it can be concluded that addition of the salts in the amounts indicated in Table 6 did not prevent release of the menthol flavorant from the gelatin microcapsules. EXAMPLE 4
Two samples were prepared as follows.
Sample 1
Moist snus was prepared by mixing sodium carbonate, potassium sulphate, sodium chloride, ethanol and water with grinded and heated moist tobacco. The amounts were as indicated in Table 8 below. The total amount of moisture of the moist snus was about 45 % by weight based on said moist snus.
3.0 g of the moist snus and 0.15 g of HPMC coated gelatin microcapsules, said microcapsules being prepared as in Example 1 , were mixed to provide the moist snus product indicated in Table 8.
The mixture was then stored in a sealed test tube in room temperature for two weeks. The composition of the moist snus product was as indicated in Table 8.
Table 8
Component Composition (wt%)
Grinded and heated, moist 62
tobacco
Sodium carbonate 2.5
Potassium sulphate 1 .1
Sodium chloride 8.5
Ethanol 0.3
Water 20.8
Microcapsules 4.8
Total: 100.0 Sample 2
Commercially available pouches consisting of snus "Skruf fresh tranbar xtra stark white slim" (Skruf Snus AB) were chopped to provide 3.0 g snus with a moisture content of about 43% which was then mixed with 0.15 g of the HPMC coated gelatin microcapsules prepared in Example 1. The mixture was then stored in a sealed test tube in room temperature for two weeks.
Samples 1 and 2 were analyzed regarding content of menthol according to the method described in Example 1. The results are indicated in Table 9.
Table 9
As can be seen from Table 9, the free flavor content of the stored Sample 1 was only 3% indicating that substantially no flavor release from the microcapsules had taken place. In contrast, the free flavor content of the stored Sample 2 was 42% indicating a significant flavor release from the microcapsules.
It can be concluded that the HPMC coated gelatin microcapsules were substantially stable upon storage in the moist snus of Sample 1 . In comparison with Sample 1 , the storage stability of the HPMC coated gelatin microcapsules in the commercially available snuff of Sample 2 was observed to be lower.
EXAMPLE 5
Microcapsules were formed in the following manner.
20.7 g of hydroxypropyl methylcellulose, type 2910, viscosity 3mPa*s (SheffCel 60HD3, purchased from Kerry) and 2.3 g of talc was mixed with 207 g of water resulting in a 230 g weight suspension.
90 g of Millicaps 1000E_1413279 (from V. MANE FILS, France) was charged in the fluid bed. The Millicaps were substantially gelatin microcapsules containing a liquid peppermint/menthol flavorant. The above prepared 230 g weight suspension with talc and dissolved hydroxypropyl methylcellulose was then sprayed on to the Millicaps
1000E_1413279. Process equipment and settings for the process as indicated in example 1 .
The formed microcapsules were then sieved through a sieve with a mesh size of 2 mm and the upper fraction was removed.
The moist snus was prepared as in example 1 . The total amount of moisture of the snus was about 46 % by weight based on said moist snuff.
The above manufactured microcapsules were mixed with the moist snus. The composition of the moist product is indicated in Table 2.
About 7 g of the above moist product were then stored in a sealed glass bottle for two weeks at room temperature.
After storage for two weeks at room temperature the above moist product consisting of moist snus and microcapsules were evaluated regarding chemical storage stability as follows.
Table 10
*The free flavor content in Table 10 was calculated as: Free flavor (%) = Average area free flavor / Average area total flavor
Analysis regarding content of menthol was performed in two batches, one for free flavor and one for total flavor. As indicated in table 10, the free flavor content of the moist snus was only 4.73% after storage 2 weeks in room temperature. It can be concluded that the HPMC-talc coated gelatin microcapsules containing the liquid flavorant did not release the flavorant to any significant extent. Thus, the HPMC-talc coated gelatin microcapsules containing the liquid flavorant are substantially storage stable in the moist snus. EXAMPLE 6
Moist snus was prepared by mixing sodium carbonate, ethanol and water with grinded and heated moist tobacco. The amounts were as indicated in Table 1 1 below. The total amount of moisture of the snus was about 46 % by weight based on said moist snus. Thus, the moist snus of the moist snus product consisted of grinded and heated moist tobacco prepared as described above, sodium carbonate, ethanol and water in amounts as indicated in Table 1 1.
Microcapsules manufactured as in Example 5 were mixed with the moist snus to provide a moist snus product. The composition of the moist snus product is indicated in Table 1 1.
Table 11
About 7 g of the above moist product were then stored in a sealed glass bottle for two weeks at room temperature.
After storage for two weeks at room temperature the above moist product consisting of moist snus and microcapsules were evaluated regarding chemical storage stability as follows.
Analysis regarding content of menthol was performed in two batches, one for free flavor and one for total flavor. As indicated in table 12, the free flavor content of the moist snus was 41 .6% after storage 2 weeks in room temperature. Table 12
*The free flavor content in Table 12 was calculated as: Free flavor (%) = Average area free flavor / Average area total flavor
As indicated above, the average area free flavor is 2699763, and the average area total flavor is 6486840. It follows that the free flavor is 2699763/6486840=41 .6%. Thus, lowering the salt content decreases the stability of the microcapsules in the moist snus.
EXAMPLE 7
Moist snus was prepared by mixing sodium chloride, sodium carbonate, ethanol and water with grinded and heated moist tobacco. The amounts were as indicated in Table 13 below. The total amount of moisture of the snus was about 46 % by weight based on said moist snus. Thus, the moist snus of the moist snus product consisted of grinded and heated moist tobacco prepared as described above, sodium chloride, sodium carbonate, ethanol and water in amounts as indicated in Table 13.
Microcapsules manufactured as in Example 5 were mixed with the moist snus to provide a moist snus product. The composition of the moist snus product is indicated in Table 13.
Table 13
About 7 g of the above moist product were then stored in a sealed glass bottle for two weeks at room temperature.
After storage for two weeks at room temperature the above moist product consisting of moist snus and microcapsules were evaluated regarding chemical storage stability as follows.
Analysis regarding content of menthol was performed in two batches, one for free flavor and one for total flavor. As indicated in table 14, the free flavor content of the moist snus was only 4.67% after storage 2 weeks in room temperature. It can be concluded that the HPMC-talc coated gelatin microcapsules containing the liquid flavorant did not release the flavorant to any significant extent. Thus, the HPMC-talc coated gelatin microcapsules containing the liquid flavorant are substantially storage stable in the moist snus when replacing potassium sulphate with sodium chloride.
Table 14
Replicate Total flavor Replicate Free flavor
Number (area) Number (area)
1 6398000 4 322942
2 5717580 5 256656
3 6201680 6 276732
Average area: 6105753 285443,3
Free flavor (%): 4,67 *The free flavor content in Table 14 was calculated as: Free flavor (%) = Average area free flavor / Average area total flavor
EXAMPLE 8
Moist snus was prepared by mixing sodium chloride, sodium carbonate, ethanol and water with grinded and heated moist tobacco. The amounts were as indicated in Table 15 below. The total amount of moisture of the snus was about 46 % by weight based on said moist snus. Thus, the moist snus of the moist snus product consisted of grinded and heated moist tobacco prepared as described above, sodium chloride, sodium carbonate, ethanol and water in amounts as indicated in Table 15.
Microcapsules manufactured as in Example 5 were mixed with the moist snus to provide a moist snus product. The composition of the moist snus product is indicated in Table 15. Table 15
About 7 g of the above moist product were then stored in a sealed glass bottle for two weeks at room temperature.
After storage for two weeks at room temperature the above moist product consisting of moist snus and microcapsules were evaluated regarding chemical storage stability as follows.
Analysis regarding content of menthol was performed in two batches, one for free flavor and one for total flavor. As indicated in table 16, the free flavor content of the moist snus was 29.1 % after storage 2 weeks in room temperature. Table 16
*The free flavor content in Table 16 was calculated as: Free flavor (%) = Average area free flavor / Average area total flavor
As indicated above, the average area free flavor is 1831060, and the average area total flavor is 6281680. It follows that the free flavor is 1831060/6281680=29.1 %. Thus, lowering the salt content decreases the stability of the microcapsules in the moist snus.
EXAMPLE 9
Moist snus was prepared by mixing sodium carbonate, sodium chloride, potassium sulphate, propylene glycole, ethanol and water with grinded and heated moist tobacco. The amounts were as indicated in Table 17 below. The total amount of moisture of the snus was about 46 % by weight based on said moist snus. Thus, the moist snus of the moist snus product consisted of grinded and heated moist tobacco prepared as described above, sodium carbonate, sodium chloride, potassium sulphate, propylene glycole, ethanol and water in amounts as indicated in Table 17.
Microcapsules manufactured as in Example 5 were mixed with the moist snus to provide a moist snus product. The composition of the moist snus product is indicated in Table 17. Table 17
About 7 g of the above moist product were then stored in a sealed glass bottle for two weeks at room temperature.
After storage for two weeks at room temperature the above moist product consisting of moist snus and microcapsules were evaluated regarding chemical storage stability as follows. Analysis regarding content of menthol was performed in two batches, one for free flavor and one for total flavor. As indicated in table 18, the free flavor content of the moist snus was only 5.3% after storage 2 weeks in room temperature. It can be concluded that the HPMC-talc coated gelatin microcapsules containing the liquid flavorant did not release the flavorant to any significant extent. Thus, the HPMC-talc coated gelatin microcapsules containing the liquid flavorant are substantially storage stable in the moist snus.
Table 18
*The free flavor content in Table 18 was calculated as: Free flavor (%) = Average area free flavor / Average area total flavor EXAMPLE 10. Measurement of conductivity of moist snus.
The following method may be used to measure the conductivity of moist snus.
Equipment: conductivity measurement apparatus, glass beaker and a magnetic stirrer. Procedure: Mix 1 .5 g of moist snus with distilled water until the total weight becomes 450.0 g. The thus obtained mixture is stirred using the magnetic stirrer at about 200 rpm for about 2 minutes. A probe of the measurement apparatus is dipped into the thus obtained mixture a couple of times until a stable conductivity value is obtained. The mixture is allowed to stand for about 1 minute. The obtained conductivity value is recorded.

Claims

An oral smokeless moist snuff product comprising:
(a) an oral smokeless moist snuff composition comprising:
- disintegrated plant material,
-one or more salts selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combination thereof, and
- water,
wherein the total amount of the one or more salts is within the range of from 15 % by weight to 35 % by weight based on the total weight of water and total weight of the one or more salts in the oral moist smokeless snuff composition,
wherein the total amount of moisture is within the range of from 35 % by weight to
60 % by weight based on the total weight of the oral smokeless moist snuff composition;
(b) particles comprising a flavorant and a cellulose-derivatized polymer selected from the group consisting of hydroxypropyl methylcellulose, hydroxypropyl cellulose, methyl cellulose and any combination thereof,
wherein the amount of said particles is within the range of from 1 % by weight to 25 % by weight based on the total weight of the oral smokeless moist snuff product.
An oral smokeless moist snuff product according to claim 1 , wherein the disintegrated plant material comprises or consists of disintegrated tobacco and/or disintegrated non-tobacco plant fibres.
An oral smokeless moist snuff product according to claim 1 or 2, wherein the one or more salts comprises or consists of sodium chloride, sodium carbonate and potassium sulphate.
An oral smokeless moist snuff product according to any one of claims 1 to 3, wherein the one or more salts comprises sodium sulphate and/or potassium sulphate and a salt selected from the group consisting of sodium chloride, sodium carbonate, potassium carbonate and any combination thereof.
5. An oral smokeless moist snuff product according to any one of claims 1 to 4, wherein the one or more salts comprises sodium carbonate, sodium chloride and optionally one or more salts selected from the group consisting of potassium carbonate, sodium sulphate, potassium sulphate, sodium lactate, potassium lactate and any combination thereof.
An oral smokeless moist snuff product according to any one of the previous claims, wherein the total amount of the one or more salts is within the range of from 15 % by weight to 25 % by weight or from 20 % by weight to 25 % by weight, based on the total weight of water and total weight of the one or more salts in the oral smokeless moist snuff composition.
An oral smokeless moist snuff product according to any one of the previous claims, wherein the amount of particles is within the range of from 5 % by weight to 25 % by weight or from 5 % by weight to 10 % by weight based on the total weight of the oral smokeless moist snuff product.
An oral smokeless moist snuff product according to any one of the previous claims, wherein the total amount of moisture is 35 % by weight, 40 % by weight, 45 % by weight, 50 % by weight, 55 % by weight or 60 % by weight based on the total weight of the oral smokeless moist snuff composition.
An oral smokeless moist snuff product according to any one of the previous claims, wherein the one or more salts is mixed with the disintegrated plant material.
10. An oral smokeless moist snuff product according to any one of the previous
claims, wherein the particles are microcapsules and/or granules.
1 1 . An oral smokeless moist snuff product according to any one of the previous
claims, wherein the flavorant is encapsulated by a coating comprising said cellulose-derivatized polymer.
12. An oral smokeless moist snuff product according to any one of the previous claims, wherein the flavorant is encapsulated by an inner coating comprising gelatine and an outer coating comprising said cellulose-derivatized polymer. 13. An oral smokeless moist snuff product according to any one of the previous
claims, wherein said cellulose-derivatized polymer comprises or consists of hydroxypropyl methylcellulose.
14. An oral smokeless moist snuff product according to any one of the previous
claims, wherein the flavor is liquid or solid and selected from the group consisting of menthol, peppermint, spearmint, liquorice, anethol, geranium, lemon oil, orange oil, grapefruit oil, bergamot oil, vanilla, coffee, coconut, almond, pecan, walnut, peanut, hazelnut, ginger, fennel, clove, anise, cardamom, coriander, basil, oregano, rosemary, thyme, sage, jasmine, lavender, wintergreen, cocoa and cumarin.
15. Method for adding a flavorant to an oral smokeless moist snuff product according to any one of the previous claims, said method comprising the steps of:
a) applying a flavorant onto at least part of one inside surface of a container for an oral smokeless moist snuff product,
b) placing the oral smokeless moist snuff product as defined in any one of claims 1 to 14 in the container, and
c) closing the container.
EP15820112.9A 2014-12-19 2015-12-18 An oral smokeless moist snuff product Active EP3232825B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
SI201530515T SI3232825T1 (en) 2014-12-19 2015-12-18 An oral smokeless moist snuff product

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP14199332 2014-12-19
EP15161679 2015-03-30
PCT/EP2015/080495 WO2016097294A1 (en) 2014-12-19 2015-12-18 An oral smokeless moist snuff product

Publications (2)

Publication Number Publication Date
EP3232825A1 true EP3232825A1 (en) 2017-10-25
EP3232825B1 EP3232825B1 (en) 2018-10-10

Family

ID=55069838

Family Applications (1)

Application Number Title Priority Date Filing Date
EP15820112.9A Active EP3232825B1 (en) 2014-12-19 2015-12-18 An oral smokeless moist snuff product

Country Status (5)

Country Link
US (1) US20170280764A1 (en)
EP (1) EP3232825B1 (en)
DK (1) DK3232825T3 (en)
SI (1) SI3232825T1 (en)
WO (1) WO2016097294A1 (en)

Families Citing this family (29)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20160157515A1 (en) 2014-12-05 2016-06-09 R.J. Reynolds Tobacco Company Smokeless tobacco pouch
JP6987782B2 (en) * 2016-04-19 2022-01-05 アルトリア クライアント サービシーズ エルエルシー Application of flavoring particles to give flavor in the filter of smoking goods
EP3544450B1 (en) * 2016-12-30 2024-07-17 Altria Client Services LLC Smokeless products containing non-tobacco plant materials
US11849752B2 (en) 2016-12-30 2023-12-26 Altria Client Services Llc Smokeless products containing non-tobacco plant materials
US11191297B2 (en) 2018-01-02 2021-12-07 Altria Client Services Llc Smokeless products containing non-tobacco plant materials
WO2018197454A1 (en) 2017-04-24 2018-11-01 Swedish Match North Europe Ab A flavoured moist oral pouched nicotine product comprising triglyceride
EP3620068A1 (en) * 2018-09-04 2020-03-11 Reemtsma Cigarettenfabriken GmbH A pouched smokeless oral product comprising at least one flavour capsule
CN109105943A (en) * 2018-09-20 2019-01-01 湖南农业大学 A kind of Lavender odor type snuff production method and its manufactured snuff
EP3897228A1 (en) 2018-12-20 2021-10-27 JT International S.A. Method of manufacturing a packaging comprising loose tobacco
US20220053813A1 (en) * 2019-02-20 2022-02-24 China Tobacco Hunan Industrial Co., Ltd. Abnormally-shaped tobacco granules and preparation method thereof, tobacco product and preparation method thereof
US11877590B2 (en) 2019-03-27 2024-01-23 Fiedler & Lundgren Ab Smokeless tobacco composition
CN111838743B (en) * 2019-04-28 2023-05-16 北京第一生物化学药业有限公司 Snuff and preparation method thereof
US11903406B2 (en) 2019-09-18 2024-02-20 American Snuff Company, Llc Method for fermenting tobacco
US11883527B2 (en) 2019-12-09 2024-01-30 Nicoventures Trading Limited Oral composition and method of manufacture
US11672862B2 (en) 2019-12-09 2023-06-13 Nicoventures Trading Limited Oral products with reduced irritation
US11969502B2 (en) 2019-12-09 2024-04-30 Nicoventures Trading Limited Oral products
US11617744B2 (en) 2019-12-09 2023-04-04 Nico Ventures Trading Limited Moist oral compositions
US11872231B2 (en) 2019-12-09 2024-01-16 Nicoventures Trading Limited Moist oral product comprising an active ingredient
AU2020403651A1 (en) 2019-12-09 2022-07-07 Nicoventures Trading Limited Oral product comprising a cannabinoid
WO2021116856A2 (en) * 2019-12-09 2021-06-17 Nicoventures Trading Limited Oral products
US20210169126A1 (en) * 2019-12-09 2021-06-10 Nicoventures Trading Limited Oral composition with salt inclusion
US11793230B2 (en) 2019-12-09 2023-10-24 Nicoventures Trading Limited Oral products with improved binding of active ingredients
US11889856B2 (en) 2019-12-09 2024-02-06 Nicoventures Trading Limited Oral foam composition
US11826462B2 (en) 2019-12-09 2023-11-28 Nicoventures Trading Limited Oral product with sustained flavor release
US11712059B2 (en) 2020-02-24 2023-08-01 Nicoventures Trading Limited Beaded tobacco material and related method of manufacture
US12016369B2 (en) 2020-04-14 2024-06-25 Nicoventures Trading Limited Regenerated cellulose substrate for aerosol delivery device
US11839602B2 (en) 2020-11-25 2023-12-12 Nicoventures Trading Limited Oral cannabinoid product with lipid component
KR20230041389A (en) * 2021-09-17 2023-03-24 주식회사 케이티앤지 Smoking articles and aerosol-generating systems
WO2024095163A1 (en) * 2022-11-01 2024-05-10 Nicoventures Trading Limited Oral composition comprising encapsulated ph adjusting agent

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2173200B1 (en) * 2007-07-23 2017-11-15 R.J.Reynolds Tobacco Company Smokeless tobacco compositions and methods for treating tobacco for use therein
US7946295B2 (en) * 2007-07-23 2011-05-24 R. J. Reynolds Tobacco Company Smokeless tobacco composition
SE0800058L (en) * 2008-01-10 2009-07-11 British American Tobacco Co Tobacco product for oral use
US8377215B2 (en) * 2008-12-18 2013-02-19 Philip Morris Usa Inc. Moist botanical pouch processing
GB2501092A (en) * 2012-04-11 2013-10-16 British American Tobacco Co Oral tobacco product

Also Published As

Publication number Publication date
WO2016097294A1 (en) 2016-06-23
US20170280764A1 (en) 2017-10-05
DK3232825T3 (en) 2018-12-17
EP3232825B1 (en) 2018-10-10
SI3232825T1 (en) 2019-02-28

Similar Documents

Publication Publication Date Title
EP3232825B1 (en) An oral smokeless moist snuff product
JP7393318B2 (en) smokeless tobacco tablets
JP7196037B2 (en) Tobacco-containing gel composition
EP3518691B1 (en) Tobacco beads
JP6568525B2 (en) Smokeless tobacco composition incorporating plant material
US8061362B2 (en) Smokeless tobacco composition
US7946295B2 (en) Smokeless tobacco composition
EP2377413B1 (en) Smokeless tobacco compositions and methods for treating tobacco for use therein
US8695609B2 (en) Smokeless tobacco composition
JP6518030B2 (en) Method for preparing a tobacco composition
WO2008056135A2 (en) A smokeless tobacco product and method for forming such a product
US20210177036A1 (en) Stimulus-responsive pouch
JP2024513466A (en) Oral pouch products
JP2024513467A (en) Liquid mixture of triglycerides and liquid nicotine
JP2024513465A (en) Encapsulated sweetener granules and their preparation method
JP2024513464A (en) Spray-dried nicotine for inclusion in oral products

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20170706

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

AX Request for extension of the european patent

Extension state: BA ME

DAV Request for validation of the european patent (deleted)
DAX Request for extension of the european patent (deleted)
GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

INTG Intention to grant announced

Effective date: 20180503

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

Ref country code: AT

Ref legal event code: REF

Ref document number: 1050189

Country of ref document: AT

Kind code of ref document: T

Effective date: 20181015

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

REG Reference to a national code

Ref country code: DE

Ref legal event code: R096

Ref document number: 602015018055

Country of ref document: DE

REG Reference to a national code

Ref country code: CH

Ref legal event code: NV

Representative=s name: VALIPAT S.A. GEVERS SA, CH

REG Reference to a national code

Ref country code: DK

Ref legal event code: T3

Effective date: 20181210

REG Reference to a national code

Ref country code: NO

Ref legal event code: T2

Effective date: 20181010

REG Reference to a national code

Ref country code: SE

Ref legal event code: TRGR

REG Reference to a national code

Ref country code: NL

Ref legal event code: MP

Effective date: 20181010

REG Reference to a national code

Ref country code: LT

Ref legal event code: MG4D

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20181010

REG Reference to a national code

Ref country code: CH

Ref legal event code: PCAR

Free format text: NEW ADDRESS: RUE DES NOYERS 11, 2000 NEUCHATEL (CH)

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: BG

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190110

Ref country code: IS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190210

Ref country code: LT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20181010

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20181010

Ref country code: PL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20181010

Ref country code: HR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20181010

Ref country code: LV

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20181010

Ref country code: ES

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20181010

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190210

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20190111

Ref country code: RS

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20181010

Ref country code: AL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20181010

REG Reference to a national code

Ref country code: DE

Ref legal event code: R097

Ref document number: 602015018055

Country of ref document: DE

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20181010

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20181218

Ref country code: MC

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20181010

Ref country code: SK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20181010

Ref country code: SM

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20181010

Ref country code: EE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20181010

Ref country code: RO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20181010

26N No opposition filed

Effective date: 20190711

REG Reference to a national code

Ref country code: IE

Ref legal event code: MM4A

REG Reference to a national code

Ref country code: BE

Ref legal event code: MM

Effective date: 20181231

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20181218

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20181231

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20181231

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20181218

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: TR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20181010

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MK

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20181010

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20181010

Ref country code: HU

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT; INVALID AB INITIO

Effective date: 20151218

REG Reference to a national code

Ref country code: AT

Ref legal event code: UEP

Ref document number: 1050189

Country of ref document: AT

Kind code of ref document: T

Effective date: 20181010

P01 Opt-out of the competence of the unified patent court (upc) registered

Effective date: 20230521

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20231213

Year of fee payment: 9

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: SI

Payment date: 20231113

Year of fee payment: 9

Ref country code: SE

Payment date: 20231220

Year of fee payment: 9

Ref country code: NO

Payment date: 20231218

Year of fee payment: 9

Ref country code: DK

Payment date: 20231212

Year of fee payment: 9

Ref country code: CZ

Payment date: 20231123

Year of fee payment: 9

Ref country code: AT

Payment date: 20231211

Year of fee payment: 9

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20240112

Year of fee payment: 9

Ref country code: CH

Payment date: 20240102

Year of fee payment: 9