Classifications

• • A—HUMAN NECESSITIES
  • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
  • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
  • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
  • A24B15/10—Chemical features of tobacco products or tobacco substitutes
  • A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
• • A—HUMAN NECESSITIES
  • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
  • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
  • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
  • A24B15/18—Treatment of tobacco products or tobacco substitutes
  • A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
  • A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
• • A—HUMAN NECESSITIES
  • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
  • A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
  • A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
  • A24B15/18—Treatment of tobacco products or tobacco substitutes
  • A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
  • A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
  • A24B15/302—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
  • A24B15/303—Plant extracts other than tobacco
• • A—HUMAN NECESSITIES
  • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
  • A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES OF CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
  • A24D1/00—Cigars; Cigarettes
  • A24D1/20—Cigarettes specially adapted for simulated smoking devices

Definitions

• the present disclosure relates to an aerosol generating material and non-combustible aerosol-provision systems comprising the aerosol generating material.
• Aerosol generating materials are typically heated, for example by a non-combustible aerosol-provision system, to form an aerosol, which may be inhaled by a consumer. Aerosol generating materials may be made from various different sources, including from tobacco material and/or non-tobacco material.
• an aerosol generating material comprising a non-tobacco botanical material which produces an aerosol when heated, the aerosol having an odour activity value (OAV) of less than about 200, wherein the non-tobacco botanical material is not rooibos.
• OAV odour activity value
• an aerosol generating rod comprising an aerosol generating material according to the first aspect.
• an article comprising the aerosol generating material according to the first aspect or the aerosol generating rod according to the second aspect.
• a delivery system comprising the aerosol generating rod according to second aspect or the article according to the third aspect.
• Figure 1 is a side-on cross-sectional view of an article for use with a non-combustible aerosol provision device.
• aerosol generating material describes a material that can generate an aerosol, for example when heated, irradiated, or energized in any other way.
• the aerosol generating materials described herein may take any suitable form and may be in reconstituted form, expanded form, cut strips, sheet form, a gathered sheet, extruded form, or any other appropriate form in the field.
• the aerosol generating material may be manufactured by any appropriate method used in the field, such as a paper-making process, a band casting method, and extruding.
• the aerosol generating material may be incorporated into an article for use with a delivery system.
• An article is sometimes referred to as a consumable throughout this disclosure.
• delivery system is intended to encompass systems that deliver at least one substance to a user and includes non-combustible aerosol provision systems that release compounds from an aerosol-generating material without combusting the aerosol-generating material, such as electronic cigarettes, tobacco heating products, and hybrid systems to generate aerosol using a combination of aerosol-generating materials.
• a "non-combustible" aerosol provision system is one where a constituent aerosol-generating material of the aerosol provision system (or component thereof) is not combusted or burned in order to facilitate delivery of at least one substance to a user.
• the delivery system is a non-combustible aerosol provision system, such as a powered non-combustible aerosol provision system.
• the non-combustible aerosol provision system can be an electronic cigarette, also known as a vaping device or electronic nicotine delivery system (END), although it is noted that the presence of nicotine in the aerosol-generating material is not a requirement.
• END electronic nicotine delivery system
• the non-combustible aerosol provision system may be an aerosol-generating material heating system, also known as a heat-not-burn system.
• An example of such a system is a tobacco heating system.
• the non-combustible aerosol provision system is a hybrid system to generate aerosol using a combination of aerosol-generating materials, one or a plurality of which may be heated.
• Each of the aerosol-generating materials may be, for example, in the form of a solid, liquid or gel and may or may not contain nicotine.
• the hybrid system comprises a liquid or gel aerosol-generating material and a solid aerosol-generating material.
• the non-combustible aerosol provision system may comprise a non-combustible aerosol provision device and a consumable for use with the non-combustible aerosol provision device.
• the non-combustible aerosol provision system such as a non-combustible aerosol provision device thereof, may comprise a power source and a controller.
• the power source may, for example, be an electric power source or an exothermic power source.
• the exothermic power source comprises a carbon substrate which may be energised so as to distribute power in the form of heat to an aerosol-generating material or to a heat transfer material in proximity to the exothermic power source.
• the non-combustible aerosol provision system comprises an area for receiving the article for use in the non-combustible aerosol-provision system, a housing, a mouthpiece, a filter and/or an aerosol-modifying agent.
• the aerosol generating material is in the form of a rod.
• the aerosol generating rod may have a total weight of between about 250 mg and about 350 mg.
• the aerosol generating rod may be wrapped in a wrapper having a permeability of less than 100 Coresta Units.
• the aerosol generating rod may have an outer circumference of at least about 19 mm, preferably between about 19 mm and about 23 mm or about 21 mm. This may facilitate insertion of the article into an aerosol generation device.
• rod is used to describe a generally cylindrical element of substantially circular, oval, or elliptical cross section.
• the aerosol generating material may comprise, or be, a continuous sheet of material.
• the sheet may be in the form of a wrapper, it may be gathered to form a gathered sheet or it may be shredded to form a shredded sheet.
• the shredded sheet may comprise one or more strands or strips of aerosol generating material.
• any water that may be present in the aerosol-generating material, or in any component thereof, is entirely disregarded for the purposes of the determination of the weight %.
• the water content of the aerosol-generating material described herein may vary according to, for example, the temperature, pressure and humidity conditions at which the compositions are maintained. The water content can be determined by Karl-Fisher analysis, as known to those skilled in the art.
• the aerosol-former material is a component that is in liquid phase, such as glycerol or propylene glycol, any component other than water is included in the weight of the aerosol-generating material.
• the aerosol generating material has a water content of between about 3% to about 15%.
• the aerosol generating material has a water content of between about 3% and about 12%, such as between about 3% and about 10%, such as between about 3% and about 9%, such as between about 3% and about 8%, such as between about 4% to about 7%, for example between about 5% and about 6%.
• the aerosol generating material comprises a water content of about 5%.
• the aerosol generating material has a filling value from about 2 cm 3 /g to about 10 cm 3 /g. In some embodiments, the aerosol generating material has a filling value of from about 3 cm 3 /g to about 8 cm 3 /g, for example the aerosol generating material may have a filling value of from about 4 cm 3 /g to about 7 cm 3 /g, such as from about 4 cm 3 /g to about 6 cm 3 /g. In some embodiments, the aerosol generating material has a filling value of about 5 cm 3 /g.
• the filling value is between about 2 cm 3 /g to about 10 cm 3 /g, for example about 5 cm 3 /g
• a consumable containing the aerosol generating material can achieve the same firmness using less material. Therefore, the overall weight of material used to achieve the same/required filling value, is less, which can provide a saving to the cost of goods.
• the article 1 comprises a mouthpiece 2, and an aerosol-generating section 3, connected to the mouthpiece 2.
• the aerosol-generating section 3 comprises the aerosol-generating material.
• the article 1 comprises a downstream end 2b and an upstream end 2a distal from the downstream end 2b.
• the aerosol generating material as described herein is provided in an aerosol generating section.
• the aerosol-generating material is circumscribed by a wrapper 5.
• the wrapper 5 is a moisture impermeable wrapper.
• the wrapper is paper, but may be made of alternative materials, such as aluminium.
• the mouthpiece 2 includes a cooling section 6, also referred to as a cooling element, positioned immediately downstream of and adjacent to the source of aerosol-generating material 3.
• the cooling section 6 is in an abutting relationship with the source of aerosol-generating material 3.
• the mouthpiece 2 also includes, in the present example, a body of material 7 downstream of the cooling section 6, and a hollow tubular element 8 downstream of the body of material 7, at the mouth end of the article 1.
• the aerosol-generating material may comprise or be in the form of an aerosol-generating film.
• the aerosol-generating film may comprise a binder, such as a gelling agent, and an aerosol former.
• a substance to be delivered and/or filler may also be present.
• the aerosol-generating film may be substantially free from botanical material.
• the aerosol-generating material is substantially tobacco free.
• the aerosol-generating film may have a thickness of about 0.015 mm to about 1 mm.
• the thickness may be in the range of about 0.05 mm, 0.1 mm or 0.15 mm to about 0.5 mm or 0.3 mm.
• the aerosol-generating film may be continuous.
• the film may comprise or be a continuous sheet of material.
• the sheet may be in the form of a wrapper, it may be gathered to form a gathered sheet or it may be shredded to form a shredded sheet.
• the shredded sheet may comprise one or more strands or strips of aerosol-generating material.
• the aerosol-generating film may be discontinuous.
• the aerosol-generating film may comprise one or more discrete portions or regions of aerosol-generating material, such as dots, stripes or lines, which may be supported on a support.
• the support may be planar or non-planar.
• the aerosol-generating film may be formed by combining a binder, such as a gelling agent, with a solvent, such as water, an aerosol-former and one or more other components, such as one or more substances to be delivered, to form a slurry and then heating the slurry to volatilise at least some of the solvent to form the aerosol-generating film.
• a binder such as a gelling agent
• a solvent such as water
• an aerosol-former such as one or more other components, such as one or more substances to be delivered
• the slurry may be heated to remove at least about 60 wt%, 70 wt%, 80 wt%, 85 wt% or 90 wt% of the solvent.
• the aerosol-generating material may comprise or be an "amorphous solid".
• the aerosol-generating materiel comprises an aerosol-generating film that is an amorphous solid.
• the amorphous solid may be a "monolithic solid".
• the amorphous solid may be substantially non-fibrous.
• the amorphous solid may be a dried gel.
• the amorphous solid is a solid material that may retain some fluid, such as liquid, within it.
• the amorphous solid may, for example, comprise from about 50wt%, 60wt% or 70wt% of amorphous solid, to about 90wt%, 95wt% or 100wt% of amorphous solid.
• the aerosol-generating film and/or amorphous solid may be substantially free from botanical material.
• the aerosol-generating film and/or amorphous solid may be substantially tobacco free.
• the non-tobacco botanical material is a solid plant/plant-based material.
• the flavour comprises menthol, spearmint and/or peppermint.
• the flavour comprises flavour components of cucumber, blueberry, citrus fruits and/or redberry.
• the flavour comprises eugenol.
• the flavour comprises flavour components extracted from tobacco.
• the flavour comprises flavour components extracted from cannabis.
• the aerosol generating material comprises two or more different non-tobacco botanical materials which have a combined OAV of less than about 200, such as less than about 150, such as less than about 125, such as less than about 100, such as less than about 75, such as less than about 50, such as less than about 30, such as less than about 25, such as less than about 20, such as less than about 10.
• the aerosol generating material comprises two or more different non-tobacco botanical materials which have a combined OAV of greater than about 200, such as greater than about 250, greater than about 300, greater than about 350, greater than about 400, greater than about 450, greater than about 500, greater than about 550, greater than about 600.
• wood fibre and wood pulp may be used to describe a cellulose material derived from a material which has little, or substantially no, noticeable aroma.
• wood fibre and wood pulp may be of similar nature to wood fibre/wood pulp used to make paper.
• Wood fibre and wood pulp are typically obtained from a non-tobacco material.
• the fibrous material has an OAV of less than about 5, such as less than about 4, less than about 3, less than about 2, less than about 1, less than about 0.5. In some embodiments, the fibrous material has an OAV of essentially zero.
• the thickness may be from about 320 ⁇ m to about 350 ⁇ m.
• the thickness may be from about 320 ⁇ m to about 340 ⁇ m.
• the thickness may be from about 325 ⁇ m to about 340 ⁇ m.
• the thickness may be from about 330 ⁇ m to about 340 ⁇ m.
• the aerosol generating material comprises a binder.
• the binder is arranged to bind the components of the aerosol generating material.
• the aerosol generating material can comprise more than one binder.
• the binders in the first composition can be the same or different.
• the binder may be selected from one or more compounds selected from the group comprising alginates, pectins, starches (and derivatives), celluloses (and derivatives), gums, silica or silicones compounds, clays, polyvinyl alcohol and combinations thereof.
• the binder comprises one or more of alginates, pectins, hydroxyethyl cellulose, hydroxypropyl cellulose, carboxymethylcellulose (CMC), pullulan, xanthan gum, guar gum, carrageenan, agarose, acacia gum, fumed silica, PDMS, sodium silicate, kaolin and polyvinyl alcohol.
• the binder comprises alginate and/or pectin or carrageenan.
• the binder comprises CMC.
• the aerosol generating material is in an extruded form.
• An extruded material is a material which is prepared by mixing components to form a mixture and extruding the mixture using an extruder equipped with an orifice, such as a shaping die.
• Extrusion may be performed using one of the main classes of extruders: screw, twin screw, sieve and basket, roll, and ram extruders.
• the mixture may be exposed to elevated pressure when forced though the orifice to form an extruded material.
• the extruded material has an elongated form and/or it may be cut into segments of a desired length as it exits the extruder. A rod-like extruded material may subsequently be cut into segments of desired length.
• the extruded material may be shaped by the orifice or die through which it is forced. In some embodiments, the extruded material is cut into pieces of desired length. The pieces formed in this way may be used as aerosol generating components or they may undergo further processing.
• the orifice or die may be shaped to provide a strand of extruded material.
• the extruded material may have the form of a cylindrical rod.
• the extruded material may have different cross-sectional shapes, including oval, polygonal (such as triangular, square, etc.), and stars.
• the extruder may be operated without applying heat to the system (for example, at room/ambient temperature) or at an elevated temperature. Where the extruder is operated at an elevated temperature, the extruder may be operated at a temperature of up to about 200 °C. After the material exits the die of the extruder, it may be cooled, for example to room temperature, to provide the extruded material.
• the mixture may be exposed to pressures ranging from about 2 bar to about 100 bar, or from about 5 bar to about 60 bar, depending on the design of the die being used.
• Flavour may be applied to the extruded material.
• the flavour may be applied by applying a film of the flavour composition onto a surface of the material, spraying the flavour composition onto the material, applying droplets of the flavour composition onto a surface of the material or submerging the material in a solution comprising the flavour composition.
• Liquids may be added to the mixture during the extrusion process.
• water may be added to the mixture, for example as a processing aid to assist dissolution or solubilisation of components of the mixture, or to aid binding or agglomeration.
• a wetting agent may be added to the mixture.
• the liquid may be an aerosol former material such as glycerol or others discussed herein, such as water.
• an aerosol former material such as glycerol or others discussed herein, such as water.
• the liquid is applied not only on the surface, but, as a result of the extruder pressure combined with the intensive mixing by high shear forces, the extruded material becomes impregnated with the liquid.
• the liquid is an aerosol former material, this can result in a high availability of the aerosol former material in the extruded material to enhance evaporation of flavour components and other components of the final aerosol-forming material.
• the liquid is water, this may assist in the extrusion process, allowing a suitable/useable extruded aerosol generating material to be formed.
• the moisture content of the mixture is from about 5 wt% to about 15 wt%, such as from about 7 wt% to about 13 wt%, such as from about 10 wt% to about 12 wt%, based on the total weight of the mixture.
• the extruded material is formed into a desired shape selected to enhance or promote the release of active and/or flavour, for example by providing a form having a large surface area per unit volume. This large surface area may be provided on the outer surface of the extruded material, for example by selecting cross-sectional shapes with large perimeter.
• the orifice or die may be shaped to provide an extruded material with inner channels.
• the presence of such inner channels provide further surface area and can enhance active and/or flavour release.
• the channel structure of the extruded aerosol generating material has enlarged inner surface area leading to improved heat and mass transfer. As a result, such components exhibit better, more uniform aerosol delivery.
• the structure with channels exhibits significantly improved strength in both the radial and axial directions, which is beneficial for the further processing of the aerosol generating material, for example when it is cut into segments and incorporated into a consumable.
• the aerosol generating material may comprise, or be, a continuous sheet of material.
• the sheet may be in the form of a shredded sheet.
• the aerosol generating material may be prepared by a papermaking process, including:
• the extract from the non-tobacco botanical material is reintroduced into the base sheet.
• the sheet comprises refined pulp produced from the non-tobacco botanical material and refined pulp from a different source, e.g. a fibrous material from a different source.
• the sheet may further comprise refined pulp obtained from wood, hemp or cotton.
• the sheet may comprise refined pulp obtained from a different non-tobacco botanical material, therefore creating a blend/mix of different non-tobacco botanical materials.
• impregnating the sheet comprises spraying a solution onto the sheet.
• the solution may be sprayed onto the sheet by an electric sprayer or using a compressed air sprayer.
• the sheet is impregnated with active by passing the sheet through a bath comprising a solution.
• the sheet may be fully submerged into the solution bath such that the sheet is impregnated with active. Submerging the sheet in a solution bath may result in greater coverage of active on the sheet compared to simply spraying the sheet with solution.
• the sheet may be passed through a solution bath and sprayed with solution.
• the sheet may be fully submerged in a solution bath, removed, and subsequently sprayed with a solution.
• the sheet may be submerged in a solution bath, removed, dried, and subsequently sprayed with solution.
• the extract, active and/or flavourant may be combined with the refined pulp in the papermaking machine, e.g. added to the slurry prior to forming the base sheet.
• the active may be dissolved in a solvent to form the solution.
• a suitable solvent system would be readily identifiable to a skilled artisan depending on the properties of the active.
• a hydrophilic active may be dissolved in an aqueous solvent.
• Suitable solvents include water.
• a lipophilic active may be dissolved in an organic solvent.
• the impregnated sheet may be dried in a drying device, such as in a commercial air/steam drier.
• the aerosol generating material may be cut into sheets, strips similar to strips of tobacco, or rolled into a roll that could be cut into webs for inclusion in a delivery system.
• two or more sheets can be combined to form a laminate.
• two or more sheets can be combined prior to drying.
• a first sheet may be combined with a second sheet made from the same non-tobacco botanical material to form a laminate.
• a first sheet may be combined with a second sheet made from a different non-tobacco botanical material to form a laminate.
• Forming a laminate made from two different non-tobacco botanical materials may provide a desirable aerosol profile for a consumer.
• a first sheet may be combined with a second sheet made from a tobacco material, such as a sheet of reconstituted tobacco. Combining a sheet made from a non-tobacco botanical material with a sheet made from tobacco material may enable the consumer to elevate the favourable/desirable aromas associated with an aerosol formed from a tobacco material.
• the aerosol generating material may comprise, or be, a continuous sheet of material.
• the sheet may be in the form of a wrapper, it may be gathered to form a gathered sheet or it may be shredded to form a shredded sheet.
• the shredded sheet may comprise one or more strands or strips of aerosol generating material.
• the strands or strips of material may be formed by shredding the sheet of aerosolisable material.
• the sheet of aerosolisable material may be cut width-wise, for example in a cross-cut type shredding process, to define a cut length for the strands or strips of aerosolisable material, in addition to a cut width.
• the cut length of the shredded aerosolisable material is preferably at least 5 mm, for instance at least 10 mm, or at least 20 mm.
• the cut length of the shredded aerosolisable material can be less than 60 mm, less than 50 mm, or less than 40 mm.
• the aerosol generating material may be prepared by combining the non-tobacco botanical material with an active and/or flavourant, a binder, and water to form a slurry.
• the slurry is subsequently processed to form a sheet of aerosolisable material.
• the slurry may be processed by band casting it.
• the slurry may be processed by forming a layer of the slurry on a surface and then drying the slurry to remove at least a portion of the water to form the sheet.
• the sheet of aerosolisable material can be cut into strips or strands of aerosolisable material.
• the strips or strands of aerosolisable material can be gathered and formed into an article for use in a non-combustible aerosol provision system.
• a suitable process for cutting the sheet of aerosolisable material and gathering it into the article is found in WO 2019/057796 .
• the aerosolisable material can be crimped prior to being gathered and formed into the article.
• the sheet of aerosol generating material is processed into a bobbin.
• This bobbin of aerosol generating material may then be fed into a shredding apparatus, to form strands/strips of aerosol generating material.
• the aerosol generating material may be subject to a second cutting step, such as in a cross-cut type shredding process in order to obtain a defined cut length.
• Pre-sized particulate non-tobacco botanical material refers to material that has been subjected to a pre-sizing step prior to combining the botanical material with the cellulose fibre to form the initial material.
• the particle size reduction device may be a milling/cutting/shredding device.
• the size reduction device may be a disc mill.
• a hammer mill, or other milling device, may alternatively be used.
• the pre-sizing step may comprise passing the non-tobacco botanical material through an appropriately sized sieve or series of sieves, and discarding, or processing to reduce the size of, any material that does not pass through the sieve or sieves, as appropriate.
• pre-sizing the non-tobacco botanical material to provide the required particle size or particle size distribution improves the quality of the produced aerosol generating material, including the organoleptic qualities of the component or product.
• Adjusting the specific particle sizes or size distribution also provides an approach for controlling and adjusting the filling power and density of the resulting aerosol generating material.
• the initial material is subjected to increased mechanical pressure and in particular also increased temperature and moisture.
• the initial material is brought to a pre-defined increased moisture content.
• the material to be processed is also subjected to an increase in temperature, which may be obtained in particular by applying heat from outside and/or by mechanically generating pressure.
• the initial material is heated to a temperature of in the range of 60-180°C, such as 100-170°C, 120-160°C, or 130-150 °C.
• This method of producing aerosol generating material has surprisingly been found to be advantageously performed at a lower expander pressure than that used in equivalent methods for processing tobacco material.
• corresponding tobacco processing methods require the use of expander pressures in the range of 35-50 bar.
• the production of equivalent materials comprising tobacco which do not include a binder typically require pressures of at least 60 bar, such as in the range of between 60 bar and 70 bar.
• this processing method may comprise pressurising the initial material to a pressure in the range of 20-35 bar.
• This pressure is much lower than that used in the production of a corresponding material comprising only tobacco.
• the use of lower pressures, such as less than 30 bar, or less than 25 bar, have been found to provide materials that are capable of carrying the greatest levels of aerosol forming materials.
• the non-tobacco botanical material and cellulose fibre are bound together to produce an aerosol generating material that may be used subsequently for the production of aerosol provision systems. This obviates the need for expensive separate processes.
• the use of smaller particles of non-tobacco botanical material in the initial material is also advantageous because it has been found to increase the filling power of the material, particularly in combination with the use of a binder.
• the processing preferably results in a product which is an aerosol generating material, in particular a fibrous and/or granular material or filler material.
• the method results in a product which is ready for consumption and can be used directly in an aerosol provision system. This is very different from producing a smokable material film (continuous material), which is more complex to produce and which still has to be cut and dried after production.
• the product obtained as a result of the present disclosure is of a size and moisture content which make it suitable for use directly as a filler material for aerosol provision systems, including tobacco heating devices.
• the shearing gap surfaces are moved relative to one another to prevent and clear blockages. This ensures that the full cross-sectional surface of the gap is used and constant physical conditions prevail at the gap, which ultimately results in a uniform product. To this end, it has also proved to be of advantage if the gap surfaces are structured or profiled, for example, having grooves.
• Non-tobacco botanical materials were dried, grinded using analytical mill (IKA A11 basic) and sifted through sieve of mesh 1.0 mm for further analysis.
• analytical mill IKA A11 basic
• CG ⁇ GC-TOFMS analysis aliquots of powdered samples (200 ⁇ 5 mg) were transferred to centrifuge tubes of 15 mL. The extraction was carried out with 5 mL of a mixture of chloroform/methanol (1:1) using sonication for 15 minutes followed by shaking at 200 rpm for 30 min. The samples were filtered throughout 0.22 ⁇ m filter (PTFE, Millipore ® , USA) and transferred to vial for analysis. The samples were analysed in triplicate.
• Consumable sticks were conditioned at 22 ⁇ 1 °C and 60 ⁇ 3 % relative humidity for 48 h to allow equilibration to occur.
• the consumable sticks were volatilized using the Glo Hyper X3 device.
• Mainstream PPA was collected using a Cerulean SM 450 (Molins, UK) smoking machine under the Canadian smoking regime, two puffs per min, 2 s puff duration, 55 mL ⁇ 0.2 mL puff volume, 30 s puff interval.
• the particulate phase from mainstream aerosol volatilized of 3 consumable sticks was collected by a 55 mm Cambridge pad and transferred to 50 ml Erlenmeyer.
• the calibration curve analyses were carried out by an Agilent 7890B gas chromatograph coupled with a 7200-series quadrupole-time-of-flight mass spectrometer (GC-QTOFMS, Agilent Technologies, USA). This system was retrofitted with a Zoex ZX2 cooled-loop GC ⁇ GC thermal modulator (Zoex Corporation, USA) - GC ⁇ GC-QTOFMS. Samples were injected in splitless mode at 250°C. For all the analyses, a non-polar 5% phenyl 95% methylpolysiloxane phase (30 m ⁇ 0.25 mm i.d.
• DB-5ms, Agilent Technologies, USA was used as the first dimension (1D) column.
• the second dimension (2D) was a mid-polar trifluoropropyl phase (10m ⁇ 0.10 mm i.d. ⁇ 0.15 ⁇ m df) (VF-200ms, Agilent Technologies, USA).
• the carrier gas was helium 1 mL min -1 .
• Chromatographic conditions were: initial temperature of 50°C (0.2 min) increased to 140°C (18.2 min) with a heating rate of 5°C min -1 ; followed by an increase to 180°C (28.2 min) with a heating rate of 4°C min -1 , increased to 250°C (52.2 min) with a heating rate of 5°C min -1 , finally increasing to 280°C with a heating rate of 5°C min -1 and a final isothermal period at 280°C for 5 min. Both columns operated at the same temperature. Modulation period, modulation duration, modulator hot jet program and modulator cold jet temperature were, respectively, 12 s, 0.6 s, 170°C, 5°C min -1 to 370°C and -90 °C. The transfer line temperature was set at 290°C. A mass spectra range was from 33 to 500 m/z and ionization energy was 70 eV. The ion source was maintained at 250°C.
• the calibration curve analyses were carried out by Agilent 7890B gas chromatograph coupled with a 5977A MSD-series mass spectrometer detector (GC-MS, Agilent Technologies, USA).
• GC-MS mass spectrometer detector
• a 1 ⁇ L sample was injected into a non-polar 5% phenyl 95% methylpolysiloxane phase (30 m ⁇ 0,25 mm i.d. ⁇ 1 ⁇ m df) (DB-5ms, Agilent Technologies, USA) capillary column. Samples were injected in splitless mode at 250 °C using helium 1 mL min -1 as carrier gas.
• Chromatographic conditions were: initial temperature of 50 °C (0.5 min) increased to 100 °C (17.17 min) with a heating rate of 3 °C min -1 ; followed by an increase to 250 °C (42.17 min) with a heating rate of 10 °C min -1 , finally increase to 280 °C with a heating rate of 5 °C min -1 and a final isothermal period at 280 °C for 5 min.
• the transfer line temperature was set at 290 °C.
• a mass spectra range was 33 to 500 m/z and ionization energy was 70 eV.
• the ion source and quadrupole were maintained at 300 °C and 150 °C respectively.
• the calibration curve analyses were carried out by Agilent 7890B gas chromatograph coupled with a 5977A MSD-series mass spectrometer detector (GC-MS, Agilent Technologies, USA).
• GC-MS mass spectrometer detector
• a 1 ⁇ L sample was injected into a high polarity nitroterephthalic acid modified polyethylene glycol phase (30 m ⁇ 0,25 mm i.d. ⁇ 0.50 ⁇ m df) (DB-FFAP, Agilent Technologies, USA) capillary column. Samples were injected in splitless mode at 250 °C using helium 1.6 mL min -1 as carrier gas.
• Chromatographic conditions were: initial temperature of 50 °C (0.5 min) increased to 100 °C (17.2 min) with a heating rate of 3 °C min -1 ; followed by increased to 230 °C (42.2 min) with a heating rate of 10 °C min -1 ; finally increase to 240 °C with a heating rate of 20 °C min -1 and a final isothermal period at 240 °C for 4min.
• the transfer line temperature was set at 260 °C.
• a mass spectra range was 33 to 500 m/z and ionization energy was 70 eV.
• the ion source and quadrupole was maintained at 300 °C and 150 °C respectively.
• GC-MS total ion chromatogram Volatile and semi-volatile chemical data (GC-MS total ion chromatogram) were converted from raw format to a structured form (mzXML extension) and aligned in time and mass dimensions. Each blob detected is deconvoluted and compared with NIST MS compound Database. In the end, each sample is represented by a volatile and semi-volatile fingerprint of compounds extracted from NIST with acceptable match factor (MF > 600), presence of two reference molecular ion (15 ppm mass error) and retention index (50 LRI).
• MF > 600 acceptable match factor
• retention index 50 LRI
• OAV odour activity values
• MATLAB MathWorks, USA
• PLS toolbox Eigenvector, USA
• Simca Umetrics, Sweden
• MS Converter ProteoWizard, USA
• TIC Total ion chromatography
• Volatile and semi-volatile chemical data were imported from Agilent Technologies MassHunter Unknowns Analysis (version B.09.00).
• the method in the software used the library NIST 2020 MS and the method was configured to identify compounds with minimum match factor of 70% and sharpness range threshold analysed was set between 10 - 25%.
• the parameters selected for batch of samples is "Component RT”, “Compound Name”, “Match Factor”, “Formula”, “CAS”, “Component Area”, “Component Height”, “Sample Name”, “File Name” and “Best Hit”. Compounds were deconvoluted and evaluated from the first hit until the fifth hit.
• the data was exported to format "(*.xlsx)" and analysed through interpretation of the fragmentation profile per compound using spectrum data analysis tools and confirmed by retention index calculated.
• OAV odour activity values

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• 2024
  • 2024-07-10 EP EP24187853.7A patent/EP4678024A1/de active Pending
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