NOVEL AEROSOL-GENERATING SUBSTRATE COMPRISING ROSMARINUS SPECIES

Abstract

An aerosol-generating article including an aerosol-generating substrate is provided, the aerosol-generating substrate formed of a homogenised rosemary material including between 1 percent by weight and 25 percent by weight rosemary particles, between 5 percent and 30 percent by weight of an aerosol former, and between 1 percent by weight and 10 percent by weight of binder, on a dry weight basis. An aerosol-generating substrate, an aerosol-generating system, and an aerosol produced upon heating of an aerosol-generating substrate, are also provided.

Claims

1.-15. (canceled)

16. An aerosol-generating article comprising an aerosol-generating substrate, the aerosol-generating substrate formed of a homogenised rosemary material comprising between 1 percent by weight and 25 percent by weight rosemary particles, between 5 percent and 30 percent by weight of an aerosol former, and between 1 percent by weight and 10 percent by weight of binder, on a dry weight basis.

17. The aerosol-generating article according to claim 16, wherein the aerosol-generating substrate comprises: at least 50 micrograms of betulinic acid per gram of the substrate, on a dry weight basis, at least 20 micrograms of rosmaridiphenol per gram of the substrate, on a dry weight basis, and at least 0.3 micrograms of 12-O-methylcarnosol per gram of the substrate, on a dry weight basis.

18. The aerosol-generating article according to claim 17, wherein an amount of betulinic acid per gram of the substrate is at least 5 times an amount of rosmaridiphenol per gram of the substrate.

19. The aerosol-generating article according to claim 16, wherein the aerosol-generating substrate comprises greater than 0.5 percent by weight of 1,8-cineole.

20. The aerosol-generating article according to claim 16, wherein upon heating of the aerosol-generating substrate according to Test Method A, an aerosol is generated comprising: at least 30 micrograms of betulinic acid per gram of the substrate, on a dry weight basis, at least 1 microgram of rosmaridiphenol per gram of the substrate, on a dry weight basis, and at least 1 microgram of 12-O-methylcarnosol per gram of the substrate, on a dry weight basis.

21. The aerosol-generating article according to claim 20, wherein an amount of betulinic acid per gram of the substrate is at least 5 times an amount of rosmaridiphenol per gram of the substrate.

22. The aerosol-generating article according to claim 16, wherein the homogenised rosemary material further comprises at least 40 percent by weight of tobacco particles, on a dry weight basis.

23. The aerosol-generating article according to claim 22, wherein the homogenised rosemary material comprises between 5 percent and 20 percent by weight of rosemary particles and between 55 percent and 70 percent by weight of tobacco particles, on a dry weight basis.

24. The aerosol-generating article according to claim 16, wherein the aerosol-generating substrate comprises one or more sheets of the homogenised rosemary material, and wherein the one or more sheets of homogenised rosemary material each individually comprise one or more of: a thickness of between 100 μm and 600 μm, or a grammage of between about 100 g/m.sup.2 and about 300 g/m.sup.2.

25. The aerosol-generating article according to claim 16, wherein the homogenised rosemary material is in the form of cast leaf.

26. The aerosol-generating article according to claim 16, wherein upon heating of the aerosol-generating substrate according to Test Method A, the aerosol generated from the aerosol-generating substrate comprises: betulinic acid in an amount of at least 0.5 micrograms per puff of aerosol, rosmaridiphenol in an amount of at least 0.01 microgram per puff of aerosol, and 12-O-methylcarnosol in an amount of at least 0.01 micrograms per puff of aerosol, and wherein a puff of aerosol has a volume of 55 millilitres as generated by a smoking machine.

27. An aerosol-generating substrate formed of a homogenised rosemary material comprising between 1 percent by weight and 25 percent by weight rosemary particles, between 5 percent and 30 percent by weight of an aerosol former, and between 1 percent by weight and 10 percent by weight of binder.

28. The aerosol-generating substrate according to claim 27, wherein the aerosol-generating substrate comprises: at least 30 micrograms of betulinic acid per gram of the substrate, on a dry weight basis, at least 1 microgram of rosmaridiphenol per gram of the substrate, on a dry weight basis, and at least 1 microgram of 12-O-methylcarnosol per gram of the substrate, on a dry weight basis.

29. An aerosol-generating system, comprising: an aerosol-generating device comprising a heating element; and an aerosol-generating article according to claim 16.

30. An aerosol produced upon heating of an aerosol-generating substrate, the aerosol comprising: betulinic acid in an amount of at least 0.5 micrograms per puff of aerosol; rosmaridiphenol in an amount of at least 0.01 microgram per puff of aerosol; and 12-O-methylcarnosol in an amount of at least 0.01 micrograms per puff of aerosol, wherein a puff of aerosol has a volume of 55 millilitres as generated by a smoking machine.

Description

[0302] Specific embodiments will be further described, by way of example only, with reference to the accompanying drawings in which:

[0303] FIG. 1 illustrates a first embodiment of a substrate of an aerosol-generating article as described herein;

[0304] FIG. 2 illustrates an aerosol-generating system comprising an aerosol-generating article and an aerosol-generating device comprising an electric heating element;

[0305] FIG. 3 illustrates an aerosol-generating system comprising an aerosol-generating article and an aerosol-generating device comprising a combustible heating element;

[0306] FIGS. 4a and 4b illustrate a second embodiment of a substrate of an aerosol-generating article as described herein;

[0307] FIG. 5 illustrates a third embodiment of a substrate of an aerosol-generating article as described herein;

[0308] FIG. 6 is a cross sectional view of filter 1050 further comprising an aerosol-modifying element, wherein

[0309] FIG. 6a illustrates the aerosol-modifying element in the form of a spherical capsule or bead within a filter plug.

[0310] FIG. 6b illustrates the aerosol-modifying element in the form of a thread within a filter plug.

[0311] FIG. 6c illustrates the aerosol-modifying element in the form of a spherical capsule within a cavity within the filter;

[0312] FIG. 7 is a cross sectional view of a plug of aerosol-generating substrate 1020 further comprising an elongate susceptor element; and

[0313] FIG. 8 illustrates an experimental set-up for collecting aerosol samples to be analysed in order to measure characteristic compounds.

[0314] FIG. 1 illustrates a heated aerosol-generating article 1000 comprising a substrate as described herein. The article 1000 comprises four elements; the aerosol-generating substrate 1020, a hollow cellulose acetate tube 1030, a spacer element 1040, and a mouthpiece filter 1050. These four elements are arranged sequentially and in coaxial alignment and are assembled by a cigarette paper 1060 to form the aerosol-generating article 1000. The article 1000 has a mouth-end 1012, which a user inserts into his or her mouth during use, and a distal end 1013 located at the opposite end of the article to the mouth end 1012. The embodiment of an aerosol-generating article illustrated in FIG. 1 is particularly suitable for use with an electrically-operated aerosol-generating device comprising a heater for heating the aerosol-generating substrate.

[0315] When assembled, the article 1000 is about 45 millimetres in length and has an outer diameter of about 7.2 millimetres and an inner diameter of about 6.9 millimetres.

[0316] The aerosol-generating substrate 1020 comprises a plug formed from a sheet of homogenised rosemary material comprising rosemary particles, either alone or in combination with tobacco particles.

[0317] A number of examples of a suitable homogenised plant material for forming the aerosol-generating substrate 1020 are shown in Table 1 below (see Samples B to D). The sheet is gathered, crimped and wrapped in a filter paper (not shown) to form the plug. The sheet includes additives, including glycerol as an aerosol former.

[0318] An aerosol-generating article 1000 as illustrated in FIG. 1 is designed to engage with an aerosol-generating device in order to be consumed. Such an aerosol-generating device includes means for heating the aerosol-generating substrate 1020 to a sufficient temperature to form an aerosol. Typically, the aerosol-generating device may comprise a heating element that surrounds the aerosol-generating article 1000 adjacent to the aerosol-generating substrate 1020, or a heating element that is inserted into the aerosol-generating substrate 1020.

[0319] Once engaged with an aerosol-generating device, a user draws on the mouth-end 1012 of the smoking article 1000 and the aerosol-generating substrate 1020 is heated to a temperature of about 375 degrees Celsius. At this temperature, volatile compounds are evolved from the aerosol-generating substrate 1020. These compounds condense to form an aerosol. The aerosol is drawn through the filter 1050 and into the user's mouth.

[0320] FIG. 2 illustrates a portion of an electrically-operated aerosol-generating system 2000 that utilises a heating blade 2100 to heat an aerosol-generating substrate 1020 of an aerosol-generating article 1000. The heating blade is mounted within an aerosol article receiving chamber of an electrically-operated aerosol-generating device 2010. The aerosol-generating device defines a plurality of air holes 2050 for allowing air to flow to the aerosol-generating article 1000. Air flow is indicated by arrows on FIG. 2. The aerosol-generating device comprises a power supply and electronics, which are not illustrated in FIG. 2. The aerosol-generating article 1000 of FIG. 2 is as described in relation to FIG. 1.

[0321] In an alternative configuration shown in FIG. 3, the aerosol-generating system is shown with a combustible heating element. While the article 1000 of FIG. 1 is intended to be consumed in conjunction with an aerosol-generating device, the article 1001 of FIG. 3 comprises a combustible heat source 1080 that may be ignited and transfer heat to the aerosol-generating substrate 1020 to form an inhalable aerosol. The combustible heat source 80 is a charcoal element that is assembled in proximity to the aerosol-generating substrate at a distal end 13 of the rod 11. Elements that are essentially the same as elements in FIG. 1 have been given the same numbering.

[0322] FIGS. 4a and 4b illustrate a second embodiment of a heated aerosol-generating article 4000a, 4000b. The aerosol-generating substrate 4020a, 4020b comprises a first downstream plug 4021 formed from of particulate plant material comprising rosemary particles, and a second upstream plug 4022 formed from particulate plant material comprising primarily tobacco particles. A suitable homogenised plant material for use in the first downstream plug is shown in Table 1 below as one of Samples B to D. A suitable homogenised plant material for use in the second upstream plug is shown in Table 1 below as Sample A. Sample A comprises only tobacco particles and is included for the purposes of comparison only.

[0323] In each of the plugs, the homogenised plant material is in the form of sheets, which are crimped and wrapped in a filter paper (not shown). The sheets both include additives, including glycerol as an aerosol former. In the embodiment shown in FIG. 4a, the plugs are combined in an abutting end to end relationship to form the rod and are of equal length of about 6 mm each. In a more preferred embodiment (not shown), the second plug is preferably longer than the first plug, for example, preferably 2 mm longer, more preferably 3 mm longer, such that the second plug is 7 or 7.5 mm in length while the first plug is 5 or 4.5 mm in length, to provide a desired ratio of tobacco to rosemary particles in the substrate. In FIG. 4b, the cellulose acetate tube support element 1030 has been omitted.

[0324] The article 4000a, 4000b, analogously to the article 1000 in FIG. 1, is particularly suitable for use with the electrically-operated aerosol-generating system 2000 comprising a heater shown in FIG. 2. Elements that are essentially the same elements in FIG. 1 have been given the same numbering. It may be envisaged by the skilled person that a combustible heat source (not shown) may be instead be used with the second embodiment in lieu of the electrical heating element, in a configuration similar to the configuration containing combustible heat source 1080 in article 1001 of FIG. 3.

[0325] FIG. 5 illustrates a third embodiment of a heated aerosol-generating article 5000. The aerosol-generating substrate 5020 comprises a rod formed from a first sheet of homogenised rosemary material formed of particulate plant material comprising a proportion of rosemary particles, and a second sheet of homogenised plant material comprising primarily cast-leaf tobacco.

[0326] A suitable homogenised rosemary material for use as the first sheet is shown in Table 1 below as one of Samples B to D. A suitable homogenised plant material for use as the second sheet is shown in Table 1 below as Sample A. Sample A comprises only tobacco particles and is included for the purposes of comparison only.

[0327] The second sheet overlies the first sheet, and the combined sheets have been crimped, gathered and at least partially wrapped in a filter paper (not shown) to form a plug that is part of the rod. Both sheets include additives, including glycerol as an aerosol former. The article 5000, analogously to the article 1000 in FIG. 1, is particularly suitable for use with the electrically-operated aerosol-generating system 2000 comprising a heater shown in FIG. 2. Elements that are essentially the same elements in FIG. 1 have been given the same numbering. It may be envisaged by the skilled person that a combustible heat source (not shown) may be instead be used with the third embodiment in lieu of the electrical heating element, in a configuration similar to the configuration containing combustible heat source 1080 in article 1001 of FIG. 3.

[0328] FIG. 6 is a cross sectional view of filter 1050 further comprising an aerosol-modifying element. In FIG. 6a, the filter 1050 further comprises an aerosol-modifying element in the form of a spherical capsule or bead 605.

[0329] In the embodiment of FIG. 6a, the capsule or bead 605 is embedded in the filter segment 601 and is surrounded on all sides by the filter material 603. In this embodiment, the capsule comprises an outer shell and an inner core, and the inner core contains a liquid flavourant. The liquid flavourant is for flavouring aerosol during use of the aerosol-generating article provided with the filter. The capsule 605 releases at least a portion of the liquid flavourant when the filter is subjected to external force, for example by squeezing by a consumer. In the embodiment shown, the capsule is generally spherical, with a substantially continuous outer shell containing the liquid flavourant.

[0330] In the embodiment of FIG. 6b, the filter segment 601 comprises a plug of filter material 603 and a central flavour-bearing thread 607 that extends axially through the plug of filter material 603 parallel to the longitudinal axis of the filter 1050. The central flavour-bearing thread 607 is of substantially the same length as the plug of filter material 603, so that the ends of the central flavour-bearing thread 607 are visible at the ends of the filter segment 601. In FIG. 6b, filter material 603 is cellulose acetate tow. The central flavour-bearing thread 607 is formed from twisted filter plug wrap and loaded with an aerosol-modifying agent.

[0331] In the embodiment of FIG. 6c, the filter segment 601 comprises more than one plug of filter material 603, 603′. Preferably, the plugs of filter material 603, 603′ are formed from cellulose acetate, such that they are able to filter the aerosol provided by the aerosol generating article. A wrapper 609 is wrapped around and connects filter plugs 603, 603′. Inside a cavity 611 is a capsule 605 comprising an outer shell and an inner core, and the inner core contains a liquid flavourant. The capsule is otherwise similar to the embodiment of FIG. 6a.

[0332] FIG. 7 is a cross sectional view of aerosol-generating substrate 1020 further comprising an elongate susceptor strip 705. The aerosol-generating substrate 1020 comprises a plug 703 formed from a sheet of homogenised rosemary material comprising tobacco particles and rosemary particles. The elongate susceptor strip 705 is embedded within the plug 703 and extends in a longitudinal direction between the upstream and downstream ends of the plug 703. During use, the elongate susceptor strip 705 heats the homogenised rosemary material by means of induction heating, as described above.

EXAMPLE

[0333] Different samples of homogenised plant material for use in an aerosol-generating substrate according to the invention, as described above with reference to the figures, may be prepared from aqueous slurries having compositions shown Table 1. Samples B to D comprise rosemary particles and tobacco particles, in accordance with the invention. Sample A comprises only tobacco particles and is included for the purposes of comparison only.

[0334] The particulate plant material in all samples A to D accounts for 75 percent of the dry weight of the homogenised plant material, with glycerol, guar gum and cellulose fibers accounting for the remaining 25 percent of the dry weight of homogenised plant material. The samples are prepared from an aqueous slurry containing between 78-79 kg of water per 100 kg of slurry.

[0335] In the table below, % DWB refers to the “dry weight base,” in this case, the percent by weight calculated relative to the dry weight of the homogenised plant material. The rosemary powder may be formed from Rosmarinus Officinalis leaves from Spain, which may be ground to a final D95=133 microns by triple impact milling.

[0336] The slurries may be casted using a casting bar (0.6 mm) on a glass plate, dried in an oven at 140 degrees Celsius for 7 minutes, and then dried in a second oven at 120 degrees Celsius for 30 seconds.

TABLE-US-00001 TABLE 1 Dry content of slurries Cellulose Rosemary Tobacco Glycerol Guar Gum fibers Sample (% DWB) (% DWB) (% DWB) (% DWB) (% DWB) A  0   75   18 3 4 B 15   60   18 3 4 C  7.5 67.5 18 3 4 D  2.5 72.5 18 3 4

[0337] For each of the samples A to D of homogenised plant material, a plug may be produced from a single continuous sheet of the homogenised plant material, the sheets each having widths of between 100 mm to 125 mm. The individual sheets preferably have a thickness of about 220 microns and a grammage of about 200 g/m.sup.2. The cut width of each sheet may be adapted based on the thickness of each sheet to produce rods of comparable volume. The sheets may be crimped to a height of 165 microns to 170 microns, and rolled into plugs having a length of about 12 mm and diameters of about 7 mm, circumscribed by a paper wrapper.

[0338] For each of the plugs, an aerosol-generating article having an overall length of about 45 mm may be formed having a structure as shown in FIG. 3 comprising, from the downstream end: a mouth end cellulose acetate filter (about 7 mm long), an aerosol spacer comprising a crimped sheet of polylactic acid polymer (about 18 mm long), a hollow acetate tube (about 8 mm long) and the plug of aerosol-generating substrate.

[0339] For a sample of homogenised rosemary material comprising rosemary particles, the characteristic compounds of the rosemary may be extracted from the plug of homogenised rosemary material using methanol as detailed above. The extract can be analysed as described above to confirm the presence of the characteristic compounds and to measure the amounts of the characteristic compounds. This may be used to confirm that the levels of characteristic compounds are within the defined ranges, as set out above. As such, the analysis can be used to provide a quality control on the aerosol-generating substrate. For example, the extract can be analysed to confirm that the levels of betulinic acid, rosmaridiphenol and 12-O-methylcarnosol are within the ranges set out below in Table 2.

TABLE-US-00002 TABLE 2 Amount of rosemary-specific compounds in the aerosol-generating substrate Minimum amount Maximum amount Characteristic (micrograms per (micrograms per Compound gram of substrate) gram of substrate) Betulinic acid 50   2000 Rosmaridiphenol 20   1000 12-O-methylcarnosol  0.3  20

[0340] Mainstream aerosols of the aerosol-generating articles incorporating aerosol-generating substrates formed from Samples A to D of homogenised plant material may be generated in accordance with Test Method A, as defined above. For each sample, the aerosol that is produced may be trapped and analysed.

[0341] As described in detail above, according to Test Method A, the aerosol-generating articles may be tested using the commercially available IQOS® heat-not-burn device tobacco heating system 2.2 holder (THS2.2 holder) from Philip Morris Products SA. The aerosol-generating articles are heated under a Health Canada machine-smoking regimen over 30 puffs with a puff volume of 55 ml, puff duration of 2 seconds and a puff interval of 30 seconds (as described in ISO/TR 19478-1:2014).

[0342] The aerosol generated during the smoking test is collected on a Cambridge filter pad and extracted with a liquid solvent. FIG. 10 shows suitable apparatus for generating and collecting the aerosol from the aerosol-generating articles.

[0343] Aerosol-generating device 111 shown in FIG. 10 is a commercially available tobacco heating device (IQOS). The contents of the mainstream aerosol generated during the Health Canada smoking test as detailed above are collected in aerosol collection chamber 113 on aerosol collection line 120. Glass fiber filter pad 140 is a 44 mm Cambridge glass fiber filter pad (CFP) in accordance with ISO 4387 and ISO 3308.

For LC-HRAM-MS Analysis

[0344] Extraction solvent 170, 170a, which in this case is methanol and internal standard (ISTD) solution, is present at a volume of 10 mL in each micro-impinger 160, 160a. The cold baths 161, 161a each contain a dry ice-isopropyl ether to maintain the micro-impingers 160, 160a each at approximately −60° C. The gas-vapour phase is trapped in the extraction solvent 170, 170a as the aerosol bubbles through micro-impingers 160, 160a. The combined solutions from the two micro-impingers are isolated as impinger-trapped gas-vapor phase solution 180 in step 181.

[0345] The CFP and the impinger-trapped gas-vapor phase solution 180 are combined in a clean Pyrex® tube in step 190. In step 200, the total particulate matter is extracted from the CFP using the impinger-trapped gas-vapor phase solution 180 (which contains methanol as a solvent) by thoroughly shaking (disintegrating the CFP), vortexing for 5 min and finally centrifuging (4500 g, 5 min, 10° C.). Aliquots (300 μL) of the reconstituted whole aerosol extract 220 were transferred into a silanized chromatographic vial and diluted with methanol (700 μL), since the extraction solvent 170, 170a already comprised internal standard (ISTD) solution. The vials were closed and mixed for 5 minutes using an Eppendorf ThermoMixer (5° C.; 2000 rpm).

[0346] Aliquots (1.5 μL) of the diluted extracts were injected and analyzed by LC-HRAM-MS in both full scan mode and data-dependent fragmentation mode for compound identification.

For GC×GC-TOFMS Analysis

[0347] As discussed above, when samples for GC×GC-TOFMS experiments are prepared, different solvents are suitable for extracting and analysing polar compounds, non-polar compounds and volatile compounds separated from whole aerosol. The experimental set-up is identical to that described with respect to sample collection for LC-HRAM-MS, with the exceptions indicated below.

Nonpolar & Polar

[0348] Extraction solvent 171,171a, is present at a volume of 10 mL and is an 80:20 v/v mixture of dichlormethane and methanol, also containing retention-index marker (RIM) compounds and stable isotopically labeled internal standards (ISTD). The cold baths 162, 162a each contain a dry ice-isopropanol mixture to maintain the micro-impingers 160, 160a each at approximately −78° C. The gas-vapor phase is trapped in the extraction solvent 171, 171a as the aerosol bubbles through micro-impingers 160, 160a. The combined solutions from the two micro-impingers are isolated as impinger-trapped gas-vapor phase solution 210 in step 182.

Nonpolar

[0349] The CFP and the impinger-trapped gas-vapor phase solution 210 are combined in a clean Pyrex® tube in step 190. In step 200, the total particulate matter is extracted from the CFP using the impinger-trapped gas-vapor phase solution 210 (which contains dichloromethane and methanol as a solvent) by thoroughly shaking (disintegrating the CFP), vortexing for 5 min and finally centrifuging (4500 g, 5 min, 10° C.) to isolate the polar and non-polar components of the whole aerosol extract 230.

[0350] In step 250, an 10 mL aliquot 240 of the whole aerosol extract 230 was taken. In step 260, a 10 mL aliquot of water is added, and the entire sample is shaken and centrifuged. The non-polar fraction 270 was separated, dried with sodium sulfate and analysed by GC×GC-TOFMS in full scan mode.

Polar

[0351] ISTD and RIM compounds were added to polar fraction 280, which was then directly analysed by GC×GC-TOFMS in full scan mode.

[0352] Each smoking replicate (n=3) comprises the accumulated trapped and reconstituted non-polar fraction 270 and polar fraction 280 for each sample

Volatile Components

[0353] Whole aerosol was trapped using two micro-impingers 160, 160a in series. Extraction solvent 172, 172a, which in this case is N,N-dimethylformamide (DMF) containing retention-index marker (RIM) compounds and stable isotopically labeled internal standards (ISTD), is present at a volume of 10 mL in each micro-impinger 160, 160a. The cold baths 161, 161a each contain a dry ice-isopropyl ether to maintain the micro-impingers 160, 160a each at approximately −60° C. The gas-vapor phase is trapped in the extraction solvent 170, 170a as the aerosol bubbles through micro-impingers 160, 160a. The combined solutions from the two micro-impingers are isolated as a volatile-containing phase 211 in step 183. The volatile-containing phase 211 is analysed separately from the other phases and injected directly into the GC×GC-TOFMS using cool-on-column injection without further preparation.

[0354] Table 3 below shows the levels of the characteristic compounds from the rosemary particles in the aerosol generated from an aerosol-generating article according to the invention including an aerosol-generating substrate formed from a homogenised rosemary material including rosemary particles.

TABLE-US-00003 TABLE 3 Content of rosemary characteristic compounds in aerosol Minimum amount Maximum amount (micrograms per (micrograms per Compound gram of substrate) gram of substrate) Betulinic acid 30 1500 Rosmaridiphenol  1  100 12-O-methylcarnosol  1  100

[0355] For example, in an aerosol generated from Sample B, relatively high levels of the characteristic compounds would be measured. The ratio of betulinic acid to rosmaridiphenol would typically be greater than 20 to 1. The levels of the characteristic compounds would therefore be indicative of the presence of rosemary particles in the sample. In contrast, for the tobacco only Sample A, which contained substantially no rosemary particles, the levels of the characteristic compounds were found to be at or close to zero.