NOVEL AEROSOL-GENERATING SUBSTRATE
20230346001 · 2023-11-02
Assignee
Inventors
- Anu AJITHKUMAR (Neuchatel, CH)
- Daniel ARNDT (Neuchatel, CH)
- Prisca CAMPANONI (Neuchatel, CH)
- Damien DE PALO (Neuchatel, CH)
- Corinne DEFOREL (Neuchatel, CH)
- Gerhard LANG (Neuchatel, CH)
- Delphine LANGLET (Neuchatel, CH)
- Jean-Pierre SCHALLER (Neuchatel, CH)
- Zoe ODOT (Neuchatel, CH)
Cpc classification
A24B15/302
HUMAN NECESSITIES
A24D1/20
HUMAN NECESSITIES
International classification
Abstract
An aerosol-generating article is provided, including an aerosol-generating substrate, the aerosol-generating substrate formed of a homogenised plant material, including: between 1 percent by weight and 65 percent by weight of non-tobacco plant particles, on a dry weight basis; between 15 percent by weight and 55 percent by weight of aerosol former, on a dry weight basis; between 5 percent by weight and 10 percent by weight of cellulose ether, on a dry weight basis; and between 5 percent by weight and 50 percent by weight of additional cellulose, on a dry weight basis, in which the additional cellulose is in a form of isolated cellulose and is not derived from the non-tobacco plant particles, and in which a ratio of additional cellulose to cellulose ether in the homogenised plant material is at least 2.
Claims
1.-19. (canceled)
20. An aerosol-generating article comprising an aerosol-generating substrate, the aerosol-generating substrate formed of a homogenised plant material, comprising: between 1 percent by weight and 65 percent by weight of non-tobacco plant particles, on a dry weight basis; between 15 percent by weight and 55 percent by weight of aerosol former, on a dry weight basis; between 5 percent by weight and 10 percent by weight of cellulose ether, on a dry weight basis; and between 5 percent by weight and 50 percent by weight of additional cellulose, on a dry weight basis, wherein the additional cellulose is in a form of isolated cellulose and is not derived from the non-tobacco plant particles, and wherein a ratio of additional cellulose to cellulose ether in the homogenised plant material is at least 2.
21. The aerosol-generating substrate according to claim 20, wherein the homogenised plant material further comprises at least 1 percent by weight of tobacco particles.
22. An aerosol-generating article comprising an aerosol-generating substrate, the aerosol-generating substrate formed of a homogenised plant material, comprising: between 1 percent by weight and 65 percent by weight of tobacco particles, on a dry weight basis; between 15 percent by weight and 55 percent by weight of aerosol former, on a dry weight basis; between 5 percent by weight and 10 percent by weight of cellulose ether, on a dry weight basis; and between 5 percent by weight and 50 percent by weight of additional cellulose, on a dry weight basis, wherein the additional cellulose is in a form of isolated cellulose and is not derived from the tobacco particles, and wherein the ratio of additional cellulose to cellulose ether in the homogenised plant material is at least 2.
23. The aerosol-generating article according to claim 20, wherein the additional cellulose comprises cellulose powder and wherein the amount of cellulose powder corresponds to at least 5 percent by weight of the homogenised plant material, on a dry weight basis.
24. The aerosol-generating article according to claim 23, wherein a ratio of cellulose powder to cellulose ether in the homogenised plant material is at least 1.5.
25. The aerosol-generating article according to claim 23, wherein the cellulose powder has at least 95 percent by weight of cellulose.
26. The aerosol-generating article according to claim 23, wherein the cellulose powder has at least 97 percent by weight of cellulose.
27. The aerosol-generating article according to claim 20, wherein the additional cellulose comprises cellulose reinforcement fibers, and wherein an amount of cellulose reinforcement fibers corresponds to at least 3 percent by weight of the homogenised plant material, on a dry weight basis.
28. The aerosol-generating article according to claim 27, wherein a ratio of cellulose reinforcement fibers to cellulose ether in the homogenised plant material is at least 1.
29. The aerosol-generating article according to claim 20, wherein the additional cellulose comprises cellulose powder and cellulose reinforcement fibers, and wherein a ratio of cellulose powder to cellulose reinforcement fibers is at least 1.5.
30. The aerosol-generating article according to claim 20, wherein the cellulose ether comprises carboxymethyl cellulose (CMC).
31. The aerosol-generating article according to claim 20, wherein a total amount of the non-tobacco plant particles or tobacco particles and the additional cellulose is no more than 75 percent by weight of the homogenised plant material, on a dry weight basis.
32. The aerosol-generating article according to claim 20, wherein the homogenised plant material comprises rosemary particles.
33. The aerosol-generating article according to claim 20, wherein the homogenised plant material comprises: between 50 percent by weight and 65 percent by weight of non-tobacco particles on a dry weight basis, and between 15 percent by weight and 25 percent by weight of aerosol former on a dry weight basis.
34. The aerosol-generating article according to claim 21, wherein the homogenised plant material comprises: between 50 percent by weight and 65 percent by weight of tobacco particles on a dry weight basis, and between 15 percent by weight and 25 percent by weight of aerosol former on a dry weight basis.
35. The aerosol-generating article according to claim 20, wherein the homogenised plant material comprises: between 10 percent by weight and 55 percent by weight of non-tobacco particles on a dry weight basis, and between 30 percent by weight and 45 percent by weight of aerosol former on a dry weight basis.
36. The aerosol-generating article according to claim 21, wherein the homogenised plant material comprises: between 10 percent by weight and 55 percent by weight of tobacco particles on a dry weight basis, and between 30 percent by weight and 45 percent by weight of aerosol former on a dry weight basis.
37. The aerosol-generating article according to claim 33, wherein the non-tobacco particles are selected from rosemary particles, star anise particles, ginger particles, clove particles, eucalyptus particles, or combinations thereof.
38. The aerosol-generating article according to claim 32, 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.
39. The aerosol-generating article according to claim 38, 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.
Description
[0276] Specific embodiments will be further described, by way of example only, with reference to the accompanying drawings in which:
[0277]
[0278]
[0279]
[0280]
[0281]
[0282]
[0283]
[0284]
[0285]
[0286]
[0287]
[0288]
[0289] 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.
[0290] The aerosol-generating substrate 1020 comprises a plug formed from a sheet of homogenised plant material comprising rosemary particles, either alone or in combination with tobacco particles.
[0291] 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.
[0292] An aerosol-generating article 1000 as illustrated in
[0293] 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.
[0294]
[0295] In an alternative configuration shown in
[0296]
[0297] 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
[0298] The article 4000a, 4000b, analogously to the article 1000 in
[0299]
[0300] A suitable homogenised plant material for use as the first sheet is shown in Table 1 below as one of Samples B to E. 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.
[0301] 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
[0302]
[0303] In the embodiment of
[0304] In the embodiment of
[0305] In the embodiment of
[0306]
EXAMPLE 1
[0307] 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, were prepared from aqueous slurries having compositions shown Table 1. Samples B to E comprise rosemary particles, in accordance with a preferred embodiment of the invention. In Samples B to D, the rosemary particles are combined with tobacco particles. Sample A comprises tobacco particles only. Sample E comprises rosemary particles only.
[0308] The particulate plant material in all samples A to E accounted for 65 percent of the dry weight of the homogenised plant material, with glycerol, CMC, cellulose powder and cellulose reinforcement fibers accounting for the remaining 35 percent of the dry weight of homogenised plant material.
[0309] 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 was formed from Rosmarinus Officinalis leaves from Spain, which was ground to a final D95=133 microns by triple impact milling. The rosemary powder was sieved to remove particles above 200 microns. In more detail, Sample E was prepared from an aqueous slurry containing: [0310] Rosemary: 17.78 kg/100 kg of slurry [0311] Glycerol: 4.50 kg/100 kg of slurry [0312] CMC: 1.25 kg/100 kg of slurry [0313] Cellulose powder: 2.50 kg/100 kg of slurry [0314] Cellulose fibres: 1.00 kg/100 kg of slurry [0315] Water: 72.97 kg/100 kg of slurry.
TABLE-US-00001 TABLE 1 Dry content of slurries Glycerol CMC Cellulose Cellulose Sam- Rosemary Tobacco (% (% powder fibers ple (% DWB) (% DWB) DWB) DWB) (% DWB) (% DWB) A 0 65 17 5 9 4 B 1 64 17 5 9 4 C 6.5 58.5 17 5 9 4 D 13 52 17 5 9 4 E 65 0 17 5 9 4
[0316] The slurries were cast using a casting bar (0.6 mm) on a glass plate, dried in an oven at 140 degrees Celsius and then dried in a second oven at 135 degrees Celsius.
[0317] For each of the samples A to E of homogenised plant material, a plug was 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 had a thickness of about 220 microns and a grammage of about 135 g/m.sup.2. The cut width of each sheet was adapted based on the thickness of each sheet to produce rods of comparable volume. The sheets were 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.
[0318] For each of the plugs, an aerosol-generating article having an overall length of about 45 mm was formed having a structure as shown in
[0319] For Sample E of homogenised plant material, for which rosemary particles make up 100 percent of the plant particles, the characteristic compounds of the rosemary were extracted from the plug of homogenised plant material using methanol as detailed above. The extract was analysed as described above to confirm the presence of the characteristic compounds and to measure the amounts of the characteristic compounds. The results of this analysis are shown below in Table 2, wherein the amounts indicated correspond to the amount per aerosol-generating article, wherein the aerosol-generating substrate of the aerosol-generating article contained 178 mg of the Sample E of homogenised plant material.
[0320] For the purposes of comparison, the amounts of the characteristic compounds present in the particulate plant material (rosemary particles) used to form Sample E are also shown. For the particulate material, the amounts indicated correspond to the amount of the characteristic compound in a sample of particulate plant material having a weight corresponding to the total weight of the particulate plant material in the aerosol-generating article containing 178 mg of Sample E.
TABLE-US-00002 TABLE 2 Amount of rosemary-specific compounds in the particulate plant material and in the aerosol-generating substrate Amount in the particulate Amount in the aerosol- Characteristic plant material generating substrate Compound (micrograms per article) (micrograms per article) Betulinic acid 717 608 Rosmaridiphenol 243 290 12-O- 5.6 3.9 methylcarnosol
[0321] For each of the samples B to D comprising a proportion of rosemary particles, the amount of the characteristic compounds can be estimated based on the values in Table 2 by assuming that the amount is present in proportion to the weight of the rosemary particles.
[0322] Mainstream aerosols of the aerosol-generating articles incorporating aerosol-generating substrates formed from Samples A to E of homogenised plant material were generated in accordance with Test Method A, as defined above. For each sample, the aerosol that was produced was trapped and analysed.
[0323] As described in detail above, according to Test Method A, the aerosol-generating articles were 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 were 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).
[0324] The aerosol generated during the smoking test was collected on a Cambridge filter pad and extracted with a liquid solvent.
[0325] Aerosol-generating device 111 shown in
For LC-HRAM-MS Analysis:
[0326] 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.
[0327] 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).
[0328] 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:
[0329] 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.
[0330] Nonpolar & Polar
[0331] 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.
[0332] Nonpolar
[0333] 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.
[0334] 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.
[0335] Polar
[0336] ISTD and RIM compounds were added to polar fraction 280, which was then directly analysed by GC×GC-TOFMS in full scan mode.
[0337] Each smoking replicate (n=3) comprises the accumulated trapped and reconstituted non-polar fraction 270 and polar fraction 280 for each sample
[0338] Volatile Components
[0339] 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.
[0340] Table 3 below shows the levels of the characteristic compounds from the rosemary particles in the aerosol generated from an aerosol-generating article incorporating Sample E of homogenised plant material, including rosemary particles only. For the purposes of comparison, Table 3 also shows the levels of the characteristic compounds in the aerosol generated from an aerosol-generating article incorporating Sample A of homogenised plant material, including tobacco particles only (and therefore not in accordance with the invention).
TABLE-US-00003 TABLE 3 Content of characteristic compounds in aerosol Sample A Sample E Sample E Sample E (micrograms (micrograms (micrograms (micrograms Compound per article) per gram) per 55 ml puff) per article) Betulinic acid 0 2275 33.75 405 Rosmaridiphenol 0 109 1.62 19.4 12-O- 0 118.5 0.68 21.1 methylcarnosol
[0341] For example, in an aerosol generated from Sample E, relatively high levels of the characteristic compounds would be measured. The ratio of betulinic acid to rosmaridiphenol would typically be greater than 20:1. Measured levels of the characteristic compounds within the ranges above would be indicative of the presence of rosemary particles in the sample and a composition of the homogenised sheet as defined above. In contrast, for the tobacco only Sample A, which contained substantially no rosemary particles, the levels of the characteristic compounds would be found to be at or close to zero.
[0342] For each of the samples B to D comprising a proportion of rosemary particles, the amount of the characteristic compounds in the aerosol can be estimated based on the values in Table 3 by assuming that the amount is present in proportion to the weight of the rosemary particles in the aerosol-generating substrate from which the aerosol is generated.
[0343] The aerosol produced by Sample E containing 65 percent by weight rosemary powder was also found to result in reduced levels of several undesired aerosol constituents when compared to the level of the aerosol in Sample A produced using 100 percent by weight tobacco based on the dry weight of the particulate plant material.
EXAMPLE 2
[0344] Sheets of homogenised plant material according to the invention were formed using the compositions shown as Recipe 1 and Recipe 2 below in Table 4. For the purposes of comparison, a third sheet of homogenised plant material using an alternative binder (and therefore not according to the invention) was formed using the composition shown as Recipe 3 below in Table 4. All of the sheets incorporated a relatively high level of rosemary particles and were formed using a cast leaf method as set out above in Example 1.
TABLE-US-00004 TABLE 4 Dry content of slurries Rosemary Guar CMC Cellulose Cellulose Sam- powder Glycerol (% (% powder fibers ple (% DWB) (% DWB) DWB) DWB) (% DWB) (% DWB) 1 57 25 0 5 10 3 2 54 35 0 5 0 6 3 75 18 3 0 0 4
[0345] The cast leaf formed from Samples 1 and 2 in accordance with the invention were both found to be homogenous in texture with a relatively uniform thickness and high tensile strength. The cast leaf could be readily removed from the casting plate and formed into a rod of aerosol-generating substrate. In contrast, the cast leaf formed from Sample 3, using a known binder instead of the combination of CMC and cellulose, was found to be porous and fragile with virtually no tensile strength. The cast leaf could not be readily detached from the casting plate and was found to fragment such that it could not be formed into a rod of aerosol-generating substrate. This example demonstrates that the use of the combination of CMC and additional cellulose in place of the guar gum binder provides a significantly improved sheet of homogenised plant material, with a greatly improved tensile strength and homogeneity.
[0346] The cast leaf formed from Sample 2 has a relatively high level of aerosol former (35 percent by weight) and is particularly suitable for use in forming the aerosol-generating substrate of an aerosol-generating article which is intended to be heated to a temperature of below 275 degrees Celsius.
[0347] When heated to a temperature of around 265 degrees Celsius, an aerosol-generating substrate produced from the cast leaf formed from Sample 2 was found to provide a significantly improved aerosol delivery compared to the cast leaf from Sample 3. In particular, the aerosol delivery was improved to a greater extent than would be expected based on the level of aerosol former alone. This demonstrates the improvement in aerosol delivery provided by incorporating the CMC binder in place of the guar gum.
EXAMPLE 3
[0348] The following homogenised plant materials according to the invention were produced using a casting leaf method as described above for Example 1, each with a different type of non-tobacco plant material. For each plant material, the composition shown below in Table 5 was used:
TABLE-US-00005 TABLE 5 Composition of homogenised plant materials Component Amount (% DWB) Plant powder 54 CMC 5 Cellulose fibers 6 Glycerol 35
[0349] The properties of the resultant homogenised plant materials are shown in Table 6 below.
TABLE-US-00006 TABLE 6 Properties of homogenised plant materials Grammage Thickness Plant powder (g/m2) (microns) Manufacturing observations Star anise 209 409 Good sheet quality. High thickness Ginger 207 221 Good sheet quality Clove 209 215 Good sheet quality Eucalyptus 197 218 Good sheet quality Rosemary 135 223 Good sheet quality
[0350] In each case, the resultant homogenised plant material was found to have an acceptable thickness and tensile strength to enable it to be incorporated into an aerosol-generating article.