WO2023161465A1 - Provision of high nicotine aerosol - Google Patents

Provision of high nicotine aerosol Download PDF

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Publication number
WO2023161465A1
WO2023161465A1 PCT/EP2023/054818 EP2023054818W WO2023161465A1 WO 2023161465 A1 WO2023161465 A1 WO 2023161465A1 EP 2023054818 W EP2023054818 W EP 2023054818W WO 2023161465 A1 WO2023161465 A1 WO 2023161465A1
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WO
WIPO (PCT)
Prior art keywords
aerosol
nicotine
acm
puffs
liquid
Prior art date
Application number
PCT/EP2023/054818
Other languages
French (fr)
Inventor
Oswaldo PEREZ
Cecile Sinkinson
Kei Yamamoto
Original Assignee
Jt International S.A.
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Filing date
Publication date
Application filed by Jt International S.A. filed Critical Jt International S.A.
Publication of WO2023161465A1 publication Critical patent/WO2023161465A1/en

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Classifications

    • 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
    • A24B15/10Chemical features of tobacco products or tobacco substitutes
    • A24B15/16Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
    • A24B15/167Chemical features of tobacco products or tobacco substitutes of tobacco substitutes in liquid or vaporisable form, e.g. liquid compositions for electronic cigarettes
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24FSMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/50Control or monitoring
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24FSMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/10Devices using liquid inhalable precursors

Definitions

  • the present invention is directed to a method and a device for delivering an aerosol to a user. More specifically, the present invention is directed to a method and a device for delivering an aerosol from an aerosol liquid heated in an aerosol generating device, wherein the aerosol liquid comprises at least 55 wt. % of propylene glycol, and wherein the delivery of aerosol is controlled by the device such that the aerosol collected mass, ACM, is at least 85 mg/25 puffs.
  • An aerosol generation device or e-cigarette, is now a mainstream product to simulate a traditional tobacco cigarette.
  • aerosol generation devices There are many types of aerosol generation devices, and the ones which still have tobacco or volatile substrate inside is one of the popular types.
  • e-cigarette There is also another type of e-cigarette, the operation method of which is to evaporate liquid to form an aerosol. Especially the e-cigarette operating with liquid is continuously growing in popularity.
  • E-cigarettes operating with liquid are usually arranged with a heating element and a liquid container, wherein when the user draws on the mouthpiece, liquid is moved from the liquid container towards the heating element, where the liquid is vaporized.
  • a benefit of aerosol liquids is that they do not require actual tobacco or can be formulated with low amounts of tobacco.
  • the flavour of the liquid formulations can more easily be controlled/ changed, and the nicotine level can be adjusted, independent of the tobacco flavour or amount of tobacco.
  • the amount of nicotine in the products was directly depending on the amount of tobacco.
  • nicotine can be added in nontobacco forms. This makes these products interesting for users that do not like the taste of tobacco or want to control the amount of nicotine they consume.
  • US 9,215,895 B2 relates to a method of delivering nicotine to a user comprising a nicotine formulation that comprises nicotine and an acid, such as pyruvic acid, salicylic acid, sorbic acid, lauric acid, levulinic acid, or benzoic acid, and a biologically acceptable liquid carrier, wherein the nicotine formulation has a pH between 2.1-6.7 and the nicotine concentration is from about 2% (w/w) to about 6% (w/w).
  • an acid such as pyruvic acid, salicylic acid, sorbic acid, lauric acid, levulinic acid, or benzoic acid
  • a biologically acceptable liquid carrier wherein the nicotine formulation has a pH between 2.1-6.7 and the nicotine concentration is from about 2% (w/w) to about 6% (w/w).
  • EP 3639813 Al relates to a liquid formulation comprising nicotine for aerosol administration.
  • the liquid formulation comprises 29-40% water, 57-68% PG and 2-6% nicotine.
  • Glycerol may be present but by no more than 5%.
  • the reduced glycerin amount allows a high nicotine content in the aerosol liquid that generates less visible aerosol (by lowering the glycerol content) and is better retained in the oral and respiratory tracts.
  • flavour intensity and in particular vapour density are two of the most desired characteristics in an aerosol liquid, it is therefore desired to provide an aerosol liquid formulation that allows for high amounts of nicotine while reducing a perceived negative sensation of the throat and nose and improving the overall smoking sensation of a user.
  • the inventors have found that in aerosol liquids with high amounts of nicotine the negative sensation can be reduced if the PG amount is kept at high levels while simultaneously controlling the aerosol collected mass, ACM, of the aerosol, such that the value of the ACM is high.
  • a 1st embodiment of the invention is directed to a method for delivering an aerosol from an aerosol liquid heated in an aerosol generating device comprising an electrical heater, wherein the aerosol liquid comprises at least 55 wt. % of propylene glycol (PG), glycerol, and at least 3 mg/ml of nicotine, and wherein the delivery of the aerosol is controlled by the device such that the total particulate matter is at least 85 mg/25 puffs, wherein the delivery of the aerosol is controlled by the device such that the aerosol collected mass, ACM, is at least 85 mg/25 puffs when the puffs are performed and the aerosol is collected by an analytical machine according to ISO 20768:2018.
  • PG propylene glycol
  • ACM aerosol collected mass
  • a ratio between PG and glycerol is at least 60:40, preferably at least 65:35 and more preferably at least 70:30; and/or at most 90:10, preferably at most 80:20 and most preferably at most 70:30.
  • a ratio of relatively high PG compared to glycerol has shown to have a positive impact on the overall flavour and volume/density of the smoke/ aerosol.
  • users of aerosol devices desire a high vapour density/volume. It has been shown that the above ratios have a particularly positive impact on the fruit and sweet taste, as well as the perception of menthol. While achieving the above effects, at the same time the above ratios of PG to glycerol do not increase the amount of irritation/dryness/off-feeling significantly.
  • the delivery of the aerosol is controlled by the device such that the ACM is at least 90 mg/ 25 puffs, preferably at least too mg/25 puffs, more preferably at least 110 mg/25 puffs, more preferably at least 115 mg/25 puffs, more preferably at least 120 mg/25 puffs, more preferably at least 125 mg/25 puffs, even more preferably at least 130 mg/25 puffs, most preferably at least 137 mg/25 puffs; and/or at most 220 mg/25 puffs, preferably at most 180 mg/25 puffs, more preferably at most 160 mg/25 puffs, particularly at most 140 mg/25 puffs and is most preferably at most 137 mg/25 puffs.
  • High values of ACM in the liquid formulation have been shown to have a positive impact on the overall flavour and volume of the smoke/ aerosol.
  • the above values have a particularly positive impact on the fruit and sweet taste, as well as the perception of menthol. While achieving the above effects, at the same time the above ratios values of ACM do not increase the amount of irritation/dryness/off-feeling. In fact, high amounts of ACM have been shown to decrease the amount of irritation/dryness/off- feeling.
  • the aerosol liquid comprises at least 60 wt. % of PG, preferably at least 65 wt. % of PG, and/or at most 90 wt. % of PG, preferably at most 80 wt. % of PG.
  • Such high amounts of PG improve the flavour intensity and the vapour density/ volume.
  • irritations caused by the nicotine decrease for menthol and fruit flavoured aerosol liquids with high amounts of PG.
  • the aerosol liquid comprises at least 6 mg/ml of nicotine, preferably at least 8 mg/ml of nicotine and more preferably at least 12 mg/ ml of nicotine; and/ or at most 59 mg/ ml of nicotine, preferably at most 40 mg/ml of nicotine, more preferably at most 20 mg/ml of nicotine and most preferably at most 18 mg/ml.
  • the above amounts of nicotine increase the desired stimulating effects for the user and thus provide an additional positive sensation for the user.
  • the aerosol liquid further comprises a flavour component in an amount between 1 and 25 wt. % of the aerosol liquid, preferably between 2 and 20 wt. %.
  • the aerosol liquid comprises at least one acid, preferably an organic acid, more preferably one or more of benzoic acid, lactic acid, tartaric acid, malic acid, most preferably a combination of benzoic acid, lactic acid and tartaric acid.
  • the acid-to-nicotine molar ratio is at least 0.1:1 preferably at least 0.2:1, and/or at most 2:1, preferably at most 1:1.
  • the flavour intensity and positive stimulation from the nicotine is not impacted by the added acids, while the negative impacts of the nicotine are reduced through the added acids.
  • the pH of the aerosol liquid is between 4 and 10, preferably between 5.5 and 8.
  • pH values provide an optimal taste sensation with less bitter taste caused by the nicotine. Therefore, such a pH range further improves an enhanced sensorial perception when inhaling the aerosol.
  • the aerosol generating device is an e-cigarette.
  • the aerosol liquid in an e-cigarette By using the aerosol liquid in an e-cigarette, it is possible to implement the aerosol generation device. This allows to consume the aerosol wherever it is desired by the user.
  • the ACM is determined gravimetrically (weighted on a scale).
  • the amount of the ACM is determined according to the test method specified in ISO 4387:2019.
  • Another embodiment of the invention is directed to a device for delivering an aerosol from an aerosol liquid, comprising an electrical heater and being configured to carry out the method according to any one of the preceding embodiments.
  • the device comprising means that allow the control of the ACM to be effectuated.
  • Fig. la shows plots of interaction profiles of an aerosol in the tobacco flavoured segment with regards to experienced discomfort of a user and various parameters of the e-liquid.
  • Fig. lb shows plots of interaction profiles of an aerosol in the menthol flavoured segment with regards to experienced discomfort of a user and various parameters of the e-liquid.
  • Fig. ic shows plots of interaction profiles of an aerosol in the fruit flavoured segment with regards to experienced discomfort of a user and various parameters of the e-liquid.
  • An aerosol generation device as described herein is any device that can be used to generate an aerosol. Such devices include e-cigarettes, vaporizers, and other devices capable of heating a component to produce an aerosol. It should be apparent for the skilled person, that the term “aerosol generation device” and “e-cigarete” as used hereinafter relate to a similar technical device. In fact, wherever the term “e-cigarete” is used, this maybe any technical feasible aerosol generation device.
  • the aerosol generation device of the present invention comprises an electrical heater for generating an aerosol by heating an aerosol liquid. Aerosol liquids may be inserted into the device through insertable cartridges or may be received directly by the aerosol generation device through means of a reservoir of the device.
  • the aerosol generating device may comprise a controller configured to control the electrical power supplied from a power source to the heater. By controlling the amount of power supplied to the heater, the amount of aerosol generated, and other characteristics of the aerosol may be controlled/steered. For example, by providing more power to the heater, more aerosol can be generated from the aerosol liquid.
  • the aerosol generating device may further comprise determination means for determining the effect of providing more power to the heater.
  • the determination means may be a temperature sensor for determining the temperature of the heating element when a certain amount of power is provided to the electrical heater.
  • the determination means may comprise a sensor configured to measure the density or other characteristics of the aerosol generated by heating the aerosol liquid.
  • the aerosol liquid has a nicotine concentration of at least 3 mg/ml. Higher nicotine concentrations are also possible. That is, the aerosol liquid may also comprise at least 6 mg/ml of nicotine, preferably at least 8 mg/ml of nicotine and more preferably at least 12 mg/ml of nicotine; and/or at most 59 mg/ml of nicotine, preferably at most 40 mg/ml of nicotine, more preferably at most 20 mg/ml of nicotine and most preferably at most 18 mg/ml.
  • the amount of nicotine in the aerosol liquid may vary depending on user preference and applicable regulations in different jurisdictions.
  • the nicotine is used to provide a stimulating effect to the user. This effect increases with the amount of nicotine in the formulation, such that high amounts of nicotine are often desired by users.
  • additives are added to the aerosol liquid.
  • one of these additives is propylene glycol, PG.
  • the PG functions as a liquid carrier in the aerosol liquid. It can reduce the negative impact of the nicotine and is known as a good flavour carrier. Therefore, an increase in the amount of PG does not only reduce the negative taste impact of the nicotine but has the additional positive effect of increasing the flavour intensity of the overall aerosol/aerosol liquid.
  • the aerosol liquid used for generating the inhalable aerosol comprises at least 55 wt. % of propylene glycol, such that high amounts of nicotine are possible in the aerosol liquid.
  • PG is also known to increase the “throat hit”.
  • the term “throat hit” relates to a strength of an experienced “pressure” in the throat of a user. Too high amounts of PG may trigger a very strong throat hit in the nose/throat area that can be perceived as irritational. Thus, it is desired to increase the amount of PG to as high an amount as possible, while keeping irritations at a minimum.
  • the aerosol liquid may also comprise further additives, such as glycerine and more particular a vegetable glycerine, VG.
  • glycerine and more particular a vegetable glycerine
  • VG a vegetable glycerine
  • One exemplary VG that may be used is the food additive E422.
  • the VG maybe replaced by a “non-vegetable glycerin” if technically feasible or if allowed by local regulations.
  • the VG is mainly used for its water binding properties, such as for its ability to bind to water particles in the ambient air to create vapour.
  • VG can be used to sweeten the liquid and to function as a carrier for added flavour components and/ or nicotine.
  • the PG/VG ratios are 50/50, 30/70 and 35/55/10, wherein 35/55/10 relates to a ratio of PG/VG/H2O.
  • the ratio of PG/VG is more in favour of the PG. That is, in exemplary embodiments the ratio of PG/VG maybe at least 60/40, preferably at least 65/30 and more preferably at least 70/30, and/or at most 90/ 10, preferably at most 80/20 and most preferably at most 70/30. It has been shown that high PG/VG ratios make it possible to provide much more nicotine to the user without additional negative impacts.
  • flavouring components may also be added to the aerosol liquid.
  • the aerosol liquids of the present invention are divided into three segments: the tobacco segment, the menthol segment and the fruit segment.
  • Each of the segments represents the dominating flavour of the aerosol liquid.
  • an aerosol liquid of the menthol segment may also have a strawberry taste; as long as the menthol perception is the dominant flavour/perception, it is classified as part of the menthol segment.
  • the aerosol liquid may also comprise at least one acid, preferably an organic acid.
  • the acid in the aerosol liquid may be any acid from the group of benzoic acid, lactic acid, tartaric acid, sorbic acid, malonic acid, gluconic acid, linoleic acid, saccharic acid, fumaric acid or any combination thereof.
  • the aerosol liquid may comprise a combination of benzoic acid, lactic acid, and tartaric acid.
  • citric acid may be used to enhance the fruit flavour
  • acids such as saccharic acid or gluconic and/ or malonic acid may enhance both the fruit and the sweet flavour.
  • Exemplary acid-to-nicotine ratios could be anything between o.i:i and 2:1.
  • the acid-to- nicotine molar ratio is 0.1:1, 0.2:1, 0.4:1 or 1:1. Such ratios maybe changing depending on other additives, such as the flavouring components.
  • the ACM conveys similar information as the total particulate matter, TPM, which is commonly used in the context of conventional cigarettes. That is, the TPM relates to the total mass of particles transported in a certain volume of smoke generated by a certain number of conventional cigarettes, whereas for an aerosol generation device the ACM relates to the mass of particles transported in a volume of aerosol generated by a certain number of puffs at the aerosol generation device, such as an e-cigarette or vaporizer.
  • the standard conditions for a routine analytical machine for e-cigarette aerosol for collecting the aerosol mass are defined in ISO 20768:2018 (similar to the Coresta Recommended Method No. 81).
  • ISO 20768:2018 defines a routine analytical machine for collecting aerosol from aerosol generating devices.
  • the ACM represents the mass of aerosol collected in an aerosol trapping system when operating a vapor product with the routine analytical vaping machine according to ISO 20768:2018 after a defined number of puffs.
  • the general definitions and conditions are defined in ISO 20768:2018.
  • the ACM is at least 85 mg/25 puffs. In further embodiments the ACM is at least 90 mg/25 puffs, preferably at least 100 mg/25 puffs, more preferably at least 110 mg/25 puffs, more preferably at least 115 mg/25 puffs, more preferably at least 125 mg/25 puffs, even more preferably at least 130 mg/25 puffs, and most preferably at least 137 mg/25 puffs, and/or at most 22omg/25 puffs, preferably at most 160 mg/25 puffs particularly at most 140 mg/25 puffs and most preferably at most 137 mg/25 puffs.
  • the pressure drop of a suction mechanism is, the puff duration, puff volume and puff frequency are specified, as well as the puff profile.
  • the puff profile indicates the flow rate measured over the time span of the puffs and shall be of a rectangular shape. That is, the puff profile shows a quick increase in flow rate to a maximum value, which is held for a certain time until the flow rate quickly decreases to a minimum value.
  • the maximum flow rate shall be 18,3 ml/s ⁇ 1.8 ml/s
  • the total duration of a puff shall be 3 s ⁇ 0,1 s
  • the puff frequency shall be one puff every 30 s ⁇ 0,5 s, i.e., 2 puffs per minute
  • the puff volume shall be 55 ml ⁇ 0,6 ml.
  • the device must be fully charged before the measurement to assure the same initial conditions for all the tested devices.
  • the suction machine that performs the puffs are also specified. That is, the machine shall include means to draw a fixed volume of air through the e- cigarette to produce a rectangular shaped profile according to the specification above.
  • the aerosol traps are specified. That is, an air filter shall be fitted between the suction machine and the e-cigarette.
  • the aerosol traps are specified as comprising an airtight filter holder, and end caps made of a non- hygroscopic material that are able to contain a filter disc of glass fibre material.
  • the glass fibre material has a thickness of 1 mm to 2 mm.
  • the filter material should retain at least 99% of all particles having a diameter of at least 0.3 pm of a dioctlyl phthalate aerosol with a linear air velocity of 140 mm/s. Wherein the pressure drop of the filter assembly shall not exceed 900 Pa at this air velocity.
  • the filter assembly shall be capable of quantitatively retaining the aerosol produced by the e-cigarette without loss. Furthermore, the filter assembly shall be chosen such that the pressure drop of the assembly does not exceed 250 Pa, when measured after the process of collecting the aerosol.
  • the aerosol collected mass is measured gravimetrically (namely: weighted on the scale) as a first assessment. This means, the total number of puffs taken by an analytical machine according to ISO 20768:2018 are recorded and the weight increase of the smoke trap after smoking a certain number of puffs is measured.
  • the ACM may then be determined according to the formula: where p is the number of puffs performed m is the mass of the filter assembly after performing p puffs m 0 is the mass of the filter assembly before performing any puffs.
  • an ACM value of 137 means that the mass of the filter assembly has increased by 137 mg after 25 puffs. Which means, that the total mass of the aerosol that is generated within 25 puffs is 137 mg.
  • the number of puffs has been chosen as 25 (this is not specified in the standard) which is a good compromise between having enough aerosol collected and having not too much mass on the filter to create an air breakthrough (which causes losses).
  • the aerosol generating device comprises means that allow the control of the ACM to be effectuated.
  • the ACM can be controlled using the controlling means. That is, the ACM may be controlled by controlling the power supplied to the heater of the aerosol generating device. For example, if more power is provided to the heater, which increases the temperature of the heater, the ACM value of the aerosol formed by heating the aerosol liquid increases. Similarly, if less power is provided to the heater, which decreases the temperature of the heater, the ACM value of the aerosol formed by heating the aerosol liquid decreases.
  • the aerosol generating device may comprise a determination means for determining the characteristics of the aerosol, such as the ACM.
  • the determination means comprises a temperature sensor
  • the ACM may be determined based on the temperature.
  • the ACM values of individual aerosol liquids may be (pre-) determined in a laboratory at various heater temperatures, using any of the methods described herein (such as ISO 20768:2018 etc.).
  • the temperature of the heater may then be measured using the temperature sensor. Based on the determined temperature, the corresponding ACM value obtained during the laboratory measurements is determined and considered as the current ACM of the generated aerosol.
  • the controller and/or the determination means may then determine whether the determined ACM value is desired or not. If it is determined that the determined ACM value is not desired, the controlling means may change the power provided to the heater and thereby change the temperature of the heater and the ACM of the generated aerosol.
  • exemplary aerosol liquid compositions with high nicotine amounts will be discussed. That is, the characteristics of various aerosol liquids with 18 mg/ml have been assessed and compared with one another. While the aerosol liquids have similar ingredients, the PG/VG ratio of the respective aerosol liquids vary. As indicated in tables la to ic, four different PG/VG ratios are compared with one another: 30/70, 40/60, 50/50 and 70/30, wherein the aerosol liquids of table la provide a tobacco taste, the aerosol liquids of table ib provide a menthol perception and the aerosol liquids of table ic provide a fruit and sweet taste.
  • each of the aerosol liquids have been consumed with an ACM of 75, 110 and 137 and compared with regards to the perceived vapour density, flavour intensity/ sweet taste and amount of irritation/dryness/off-feeling.
  • results shown in table la indicate that the amount of aerosol vapour increases with both the PG/VG ratio and the ACM. That is with a constant ACM of 75, the vapour density increases from “lowest” to “mid” for increasing PG/VG ratios. At a constant ACM of 110 the vapour densities increase from “low-mid” to “mid-high” for increasing PG/VG ratios and for a constant ACM of 137 the vapour density increases from “mid” to “high” for increasing PG/VG ratios. Similarly, with a constant PG/VG ratio, the vapour density increases with an increase in ACM.
  • vapour density increases from “lowest” to “mid” with increasing ACM values and at a PG/VG ratio of 80/30 the vapour density increases from “mid” to “high” for increasing ACM values.
  • Table la the vapour density increases from “lowest” to “mid” with increasing ACM values and at a PG/VG ratio of 80/30 the vapour density increases from “mid” to “high” for increasing ACM values.
  • flavour intensity/ sweet taste was also in favour of high ACM. It was noticed that the irritation experienced by a user was the lowest for low PG/VG ratio and high ACM. This is not surprising as high PG is known to increase irritation. However, it was also shown, that high PG/VG ratios are still not drastically increasing the irritation/dryness perception when the ACM is also kept at a high level.
  • flavour/vapour density/irritation perception For the tobacco flavoured aerosol liquids is could be shown that a combination of high ACM and high PG/VG ratio provide surprisingly well flavour/vapour density/irritation perception to a user.
  • the perceived flavour intensity and vapour density was the highest for a PG/VG ratio of 70/30 and an ACM value of 137, while the total irritation was kept at a medium range which is acceptable for such a significant increase in vapour density/ flavour intensity/ sweet taste.
  • Table ib relates to the same test performed for menthol perception aerosol liquids.
  • the results are rather similar, when compared to the tobacco flavoured aerosol liquid. That is, the vapour density increases with the PG/VG ratio and increases with the ACM. Similarly, the flavour intensity/ sweet taste and the cooling experience from the menthol increases with an increase in ACM, and with an increase in PG/VG ratio. Furthermore, the irritation/dryness experience by a user does not exceed a medium level and is tolerable for such a significant increase in vapour density and flavour intensity/ sweet taste/cooling perception. Optimal results with an acceptable amount of irritation were achieved with an ACM of 137 and a PG/VG ratio of 70/30.
  • the irritation/dryness perception decreases for increasing ACM values. That is, an ACM value of 75 results in “high” irritation/dryness perception, whereas an ACM value of no triggers a “mid-high” irritation/dryness perception and an ACM value of 137 triggers only “medium” irritation/dryness perception. Therefore, for fruit and/or sweet flavoured aerosol liquids high ACM values and high PG/VG ratios provide surprisingly beneficial aerosol characteristics for a consumer.
  • a PG/VG ratio of 70/30 and an ACM value of 137 shows the best results for flavour intensity and vapour density.
  • Figures la to ic show plots of the interaction profiles. That is, the amount of perceived discomfort, such as irritation/dryness with respect to the three parameters: amount of nicotine, the ratio of PG/VG and the ACM value.
  • Each of the figures la to ic show a 3x3 plot, wherein each column resembles one changing parameter, and each row resembles two constant values of the respective parameter. Therefore, the 3x3 plot shows the interaction profile of perceived irritation of a user if one isolated component changes. That is, in figures la to ic, column 1 shows the impact on the perceived irritation when only the amount of nicotine is changed, wherein column 2 shows the results of only changing the PG/VG ratio and column 3 shows the respective perceived irritation if only the ACM is changed.
  • row 1 of figures la to ic show the graphs of an aerosol liquid with of o mg/ ml and a liquid with 12 mg/ ml of nicotine in accordance with changing the PG/VG ratio (row 1, column 2) and the ACM value (row 1, column 3).
  • Row 2 of Figures la to ic shows graphs of a constant PG/VG ratio of 85 and a constant PG/VG ratio of 50 in accordance with changing nicotine amounts (row 2, column 1) and changing ACM (row 2, column 3) and row 3 shows the graphs for a constant PTM of 85 and a constant ACM of 137 in accordance with changing amounts of nicotine (row 3, column 1) and different ratios of PG/VG (rows, column 2).
  • the graphs are plotted with regards to the perceived discomfort of a user.
  • the perceived discomfort is normalized to a range of -0,75 to 1,25, wherein - 0,75 indicates the minimum perceived discomfort (irritation/dryness/off-feel) and 1,25 indicates the maximum perceived discomfort of a user.
  • column 1 of the plot of Fig. la shows that for tobacco flavoured aerosol liquids the discomfort increases with an increase in both nicotine and PG/VG ratio (column 1, row 2) and is somewhat similar for varying ACM values (column 1, row 3).
  • Column 2 of Fig. la indicates that for high nicotine levels, the irritation slightly increases with an increase of the PG/VG ratio (column 2, row 1) and decreases for high ACM values (column 2, row 3).
  • Fig. la indicates that the negative perception of nicotine increases if only the PG/VG ratio increases. Furthermore, it indicates that the irritation caused by high PG/VG ratios decreases with an increase of ACM. From this, it can be concluded that even if increasing only the PG/VG ratio could have positive benefits on vapour density/ flavour intensity, the amount of irritation might also increase. Thus, only if parallel to an increase of the PG/VG ratio the ACM increases can the positive effects be achieved while the irritation is at least kept at a constant amount. This observation confirms the results shown in table la.
  • Figure lb shows the interaction profile for aerosol liquids in the menthol segment.
  • the plots of column 1 of Fig. lb indicate that the perceived discomfort for increasing nicotine amounts is similar for high and low PG/VG ratios and high and low ACM values.
  • the plots of column 2 of Fig. lb indicate that the irritation for high nicotine liquids decreases with an increase of PG/VG (column 2, rowi) and slightly increases for high ACM values, whereas the irritation reduces with increasing PG/VG values for low ACM values (columns 2, rows).
  • column 3 indicates that the perceived negative effect of either nicotine or high PG/VG reduces with an increase of ACM.
  • Fig. ic shows that for the fruit segment, the optimal PG/VG ratio appears to be 70/30.
  • increasing amounts of ACM provide a strong positive effect for high nicotine formulations.
  • test results of Figs, la to ic show that in the tobacco segment the additional irritation caused by high PG/VG ratios at high nicotine levels can be mitigated through high ACM values. Therefore, it is possible to provide high nicotine tobacco flavoured aerosol liquids without the negative sensations caused by the nicotine if both the ACM and the PG/VG ratio are high.
  • one preferred embodiment of the invention is to use a PG/VG ratio of 70/30 and an ACM value of 137.
  • this combination shows the best overall results and in particular the best results in the fruit segment.
  • other PG/VG ratios and ACM values could be preferred.
  • a PG/VG ratio of 85/ 15 could be better suited for some applications, as indicated in Fig. ib.

Abstract

The invention is directed to a method and a device to provide an aerosol to a user from an aerosol liquid heated in an aerosol generating device comprising an electrical heater, wherein the aerosol liquid comprises at least 55 wt. % of propylene glycol, PG, glycerol, and at least 3 mg/ml of nicotine. The delivery of the aerosol is controlled by the device such that the aerosol collected mass, ACM, is at least 85 mg/25 puffs when the puffs are performed and the aerosol is collected by an analytical machine according to ISO 20768:2018.

Description

PROVISION OF HIGH NICOTINE AEROSOL
TECHNICAL FIELD
The present invention is directed to a method and a device for delivering an aerosol to a user. More specifically, the present invention is directed to a method and a device for delivering an aerosol from an aerosol liquid heated in an aerosol generating device, wherein the aerosol liquid comprises at least 55 wt. % of propylene glycol, and wherein the delivery of aerosol is controlled by the device such that the aerosol collected mass, ACM, is at least 85 mg/25 puffs.
BACKGROUND
An aerosol generation device, or e-cigarette, is now a mainstream product to simulate a traditional tobacco cigarette. There are many types of aerosol generation devices, and the ones which still have tobacco or volatile substrate inside is one of the popular types. There is also another type of e-cigarette, the operation method of which is to evaporate liquid to form an aerosol. Especially the e-cigarette operating with liquid is continuously growing in popularity.
E-cigarettes operating with liquid are usually arranged with a heating element and a liquid container, wherein when the user draws on the mouthpiece, liquid is moved from the liquid container towards the heating element, where the liquid is vaporized.
A benefit of aerosol liquids is that they do not require actual tobacco or can be formulated with low amounts of tobacco. Thus, the flavour of the liquid formulations can more easily be controlled/ changed, and the nicotine level can be adjusted, independent of the tobacco flavour or amount of tobacco. Furthermore, in traditional tobacco products the amount of nicotine in the products was directly depending on the amount of tobacco. In aerosol liquid formulations, nicotine can be added in nontobacco forms. This makes these products interesting for users that do not like the taste of tobacco or want to control the amount of nicotine they consume.
There is a high desire to provide a liquid formulation that provides an improved sensory experience through a high smoke density and a good taste experience, without any discomfort, such as irritations in the mouth and nose area, when inhaling the product. In particular, when formulated with high amounts of nicotine, the smoke tends to cause irritations of the mouth and the nose area. To mitigate this negative sensation, aerosol liquids have been formulated with relatively high amounts of organic acids and high levels of glycerol, which tend to reduce the negative effects of the nicotine.
US 9,215,895 B2 relates to a method of delivering nicotine to a user comprising a nicotine formulation that comprises nicotine and an acid, such as pyruvic acid, salicylic acid, sorbic acid, lauric acid, levulinic acid, or benzoic acid, and a biologically acceptable liquid carrier, wherein the nicotine formulation has a pH between 2.1-6.7 and the nicotine concentration is from about 2% (w/w) to about 6% (w/w).
While such high amounts of organic acids seem to reduce the irritation caused by the nicotine, the flavour intensity and vapour density decreases. To increase the amount of nicotine whilst maintaining a high flavour intensity and a sweet taste, high levels of propylene glycol, PG, are used in aerosol liquids. However, this also increases irritation of the throat and nose area.
EP 3639813 Al relates to a liquid formulation comprising nicotine for aerosol administration. The liquid formulation comprises 29-40% water, 57-68% PG and 2-6% nicotine. Glycerol may be present but by no more than 5%. The reduced glycerin amount allows a high nicotine content in the aerosol liquid that generates less visible aerosol (by lowering the glycerol content) and is better retained in the oral and respiratory tracts.
Whilst irritations seem to be reduced by lowering the glycerol content, and the overall flavour intensity seems to increase, the vapour density significantly decreases.
Since flavour intensity and in particular vapour density are two of the most desired characteristics in an aerosol liquid, it is therefore desired to provide an aerosol liquid formulation that allows for high amounts of nicotine while reducing a perceived negative sensation of the throat and nose and improving the overall smoking sensation of a user.
SUMMARY OF THE INVENTION
The inventors have found that in aerosol liquids with high amounts of nicotine the negative sensation can be reduced if the PG amount is kept at high levels while simultaneously controlling the aerosol collected mass, ACM, of the aerosol, such that the value of the ACM is high.
Hence, a 1st embodiment of the invention is directed to a method for delivering an aerosol from an aerosol liquid heated in an aerosol generating device comprising an electrical heater, wherein the aerosol liquid comprises at least 55 wt. % of propylene glycol (PG), glycerol, and at least 3 mg/ml of nicotine, and wherein the delivery of the aerosol is controlled by the device such that the total particulate matter is at least 85 mg/25 puffs, wherein the delivery of the aerosol is controlled by the device such that the aerosol collected mass, ACM, is at least 85 mg/25 puffs when the puffs are performed and the aerosol is collected by an analytical machine according to ISO 20768:2018.
With the above, it is possible to have a liquid with high amounts of nicotine whilst the perceived negative throat and mouth sensation of a user inhaling the aerosol is reduced. That is, high amounts of nicotine tend to provide a bitter taste that causes throat and nose irritation. The high ACM increases the sensorial profile (taste and feel) of the inhaled aerosol while high amounts of PG provide good vapour density and serve as a good flavour carrier. In fact, the combination of high ACM and high PG has shown to have a surprisingly positive effect on the overall sensation perceived by the user inhaling the high nicotine aerosol.
According to a 2nd embodiment, in the 1st embodiment, a ratio between PG and glycerol is at least 60:40, preferably at least 65:35 and more preferably at least 70:30; and/or at most 90:10, preferably at most 80:20 and most preferably at most 70:30.
A ratio of relatively high PG compared to glycerol has shown to have a positive impact on the overall flavour and volume/density of the smoke/ aerosol. Generally, users of aerosol devices desire a high vapour density/volume. It has been shown that the above ratios have a particularly positive impact on the fruit and sweet taste, as well as the perception of menthol. While achieving the above effects, at the same time the above ratios of PG to glycerol do not increase the amount of irritation/dryness/off-feeling significantly.
According to a 3rd embodiment, in any of the preceding embodiments, the delivery of the aerosol is controlled by the device such that the ACM is at least 90 mg/ 25 puffs, preferably at least too mg/25 puffs, more preferably at least 110 mg/25 puffs, more preferably at least 115 mg/25 puffs, more preferably at least 120 mg/25 puffs, more preferably at least 125 mg/25 puffs, even more preferably at least 130 mg/25 puffs, most preferably at least 137 mg/25 puffs; and/or at most 220 mg/25 puffs, preferably at most 180 mg/25 puffs, more preferably at most 160 mg/25 puffs, particularly at most 140 mg/25 puffs and is most preferably at most 137 mg/25 puffs.
High values of ACM in the liquid formulation have been shown to have a positive impact on the overall flavour and volume of the smoke/ aerosol. The above values have a particularly positive impact on the fruit and sweet taste, as well as the perception of menthol. While achieving the above effects, at the same time the above ratios values of ACM do not increase the amount of irritation/dryness/off-feeling. In fact, high amounts of ACM have been shown to decrease the amount of irritation/dryness/off- feeling.
According to a 4th embodiment, in any of the preceding embodiments, the aerosol liquid comprises at least 60 wt. % of PG, preferably at least 65 wt. % of PG, and/or at most 90 wt. % of PG, preferably at most 80 wt. % of PG.
Such high amounts of PG improve the flavour intensity and the vapour density/ volume. In addition, irritations caused by the nicotine decrease for menthol and fruit flavoured aerosol liquids with high amounts of PG.
According to a 5th embodiment, in any of the preceding embodiments, the aerosol liquid comprises at least 6 mg/ml of nicotine, preferably at least 8 mg/ml of nicotine and more preferably at least 12 mg/ ml of nicotine; and/ or at most 59 mg/ ml of nicotine, preferably at most 40 mg/ml of nicotine, more preferably at most 20 mg/ml of nicotine and most preferably at most 18 mg/ml.
The above amounts of nicotine increase the desired stimulating effects for the user and thus provide an additional positive sensation for the user.
According to 6th embodiment, in any of the preceding embodiments, the aerosol liquid further comprises a flavour component in an amount between 1 and 25 wt. % of the aerosol liquid, preferably between 2 and 20 wt. %.
With the above flavour agents, it is possible to provide an aerosol liquid in any desired taste. Such flavoured aerosol liquids allow users who dislike the tobacco flavour to consume an aerosol. According to a 7th embodiment, in any of the preceding embodiments, the aerosol liquid comprises at least one acid, preferably an organic acid, more preferably one or more of benzoic acid, lactic acid, tartaric acid, malic acid, most preferably a combination of benzoic acid, lactic acid and tartaric acid.
The addition of the above-listed organic acids allows to further decrease negative sensations perceived by the user through high amounts of nicotine.
According to an 8th embodiment, in the preceding embodiment, the acid-to-nicotine molar ratio is at least 0.1:1 preferably at least 0.2:1, and/or at most 2:1, preferably at most 1:1.
By keeping the acid-to-nicotine molar ratio rather low, the flavour intensity and positive stimulation from the nicotine is not impacted by the added acids, while the negative impacts of the nicotine are reduced through the added acids.
According to a 9th embodiment, in any of the preceding embodiments, the pH of the aerosol liquid is between 4 and 10, preferably between 5.5 and 8.
It has been shown that such pH values provide an optimal taste sensation with less bitter taste caused by the nicotine. Therefore, such a pH range further improves an enhanced sensorial perception when inhaling the aerosol.
According to a 10th embodiment, in any of the preceding embodiments, the aerosol generating device is an e-cigarette.
By using the aerosol liquid in an e-cigarette, it is possible to implement the aerosol generation device. This allows to consume the aerosol wherever it is desired by the user.
According to an 11th embodiment, in any of the preceding embodiments, the ACM is determined gravimetrically (weighted on a scale).
By weighting the aerosol mass that is collected in the analytical machine, it is possible to easy determine the total mass of the aerosol that is generated after a certain number of puffs.
According to a 12th embodiment, in any of the preceding embodiments, the ACM is determined according to the formular: ACM=m/p, wherein m is the weight of the aerosol mass collected by the analytical machine, and p is the total amounts of puffs. By dividing the total collected aerosol mass by the number of puffs, a qualitative statement can be made about the aerosol produced per puff, and in particular about the density of the aerosol or at least the aerosol density perceived by a user.
According to a 13th embodiment, in any one of the preceding embodiments, the amount of the ACM is determined according to the test method specified in ISO 4387:2019.
By using specifically defined tests and machines for determining the ACM, it is ensured that the tests are repeatable, and obtained ACM values are comparable.
Another embodiment of the invention is directed to a device for delivering an aerosol from an aerosol liquid, comprising an electrical heater and being configured to carry out the method according to any one of the preceding embodiments. Preferably, the device comprising means that allow the control of the ACM to be effectuated.
BRIEF DESCRIPTION OF THE DRAWINGS
The following detailed description makes reference to the accompanying drawings, which are now briefly described.
Fig. la shows plots of interaction profiles of an aerosol in the tobacco flavoured segment with regards to experienced discomfort of a user and various parameters of the e-liquid.
Fig. lb shows plots of interaction profiles of an aerosol in the menthol flavoured segment with regards to experienced discomfort of a user and various parameters of the e-liquid.
Fig. ic shows plots of interaction profiles of an aerosol in the fruit flavoured segment with regards to experienced discomfort of a user and various parameters of the e-liquid.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Preferred embodiments of the present invention are described hereinafter with reference to the drawings.
An aerosol generation device as described herein is any device that can be used to generate an aerosol. Such devices include e-cigarettes, vaporizers, and other devices capable of heating a component to produce an aerosol. It should be apparent for the skilled person, that the term “aerosol generation device” and “e-cigarete” as used hereinafter relate to a similar technical device. In fact, wherever the term “e-cigarete” is used, this maybe any technical feasible aerosol generation device.
The aerosol generation device of the present invention comprises an electrical heater for generating an aerosol by heating an aerosol liquid. Aerosol liquids may be inserted into the device through insertable cartridges or may be received directly by the aerosol generation device through means of a reservoir of the device. The aerosol generating device may comprise a controller configured to control the electrical power supplied from a power source to the heater. By controlling the amount of power supplied to the heater, the amount of aerosol generated, and other characteristics of the aerosol may be controlled/steered. For example, by providing more power to the heater, more aerosol can be generated from the aerosol liquid. The aerosol generating device may further comprise determination means for determining the effect of providing more power to the heater. For example, the determination means may be a temperature sensor for determining the temperature of the heating element when a certain amount of power is provided to the electrical heater. In another example, the determination means may comprise a sensor configured to measure the density or other characteristics of the aerosol generated by heating the aerosol liquid.
In a preferred embodiment, the aerosol liquid has a nicotine concentration of at least 3 mg/ml. Higher nicotine concentrations are also possible. That is, the aerosol liquid may also comprise at least 6 mg/ml of nicotine, preferably at least 8 mg/ml of nicotine and more preferably at least 12 mg/ml of nicotine; and/or at most 59 mg/ml of nicotine, preferably at most 40 mg/ml of nicotine, more preferably at most 20 mg/ml of nicotine and most preferably at most 18 mg/ml.
The amount of nicotine in the aerosol liquid may vary depending on user preference and applicable regulations in different jurisdictions. In aerosol liquids, the nicotine is used to provide a stimulating effect to the user. This effect increases with the amount of nicotine in the formulation, such that high amounts of nicotine are often desired by users.
However, nicotine itself has a bitter taste. In particular in high nicotine formulations, this can have a negative impact on the smoking experience. The effect of high amounts of nicotine can even be as bad as triggering irritations in the nose and throat area. For this reason, additives are added to the aerosol liquid. In the preferred embodiment, one of these additives is propylene glycol, PG. The PG functions as a liquid carrier in the aerosol liquid. It can reduce the negative impact of the nicotine and is known as a good flavour carrier. Therefore, an increase in the amount of PG does not only reduce the negative taste impact of the nicotine but has the additional positive effect of increasing the flavour intensity of the overall aerosol/aerosol liquid.
One possible PG compound that could be used in the aerosol liquid is the food additive E1520. The aerosol liquid used for generating the inhalable aerosol comprises at least 55 wt. % of propylene glycol, such that high amounts of nicotine are possible in the aerosol liquid. Such high amounts of PG already mitigate most of the negative effects of high amounts of nicotine. However, PG is also known to increase the “throat hit”. The term “throat hit” relates to a strength of an experienced “pressure” in the throat of a user. Too high amounts of PG may trigger a very strong throat hit in the nose/throat area that can be perceived as irritational. Thus, it is desired to increase the amount of PG to as high an amount as possible, while keeping irritations at a minimum. The inventors found out that the amount of PG could even be as high as 60 wt. %, and in more preferred embodiments as high as 70 and up to 80 wt. % before a significant increase in irritations is perceived by a user.
In preferred embodiments, the aerosol liquid may also comprise further additives, such as glycerine and more particular a vegetable glycerine, VG. One exemplary VG that may be used is the food additive E422. The VG maybe replaced by a “non-vegetable glycerin” if technically feasible or if allowed by local regulations. The VG is mainly used for its water binding properties, such as for its ability to bind to water particles in the ambient air to create vapour. Furthermore, VG can be used to sweeten the liquid and to function as a carrier for added flavour components and/ or nicotine.
In some embodiments, the PG/VG ratios are 50/50, 30/70 and 35/55/10, wherein 35/55/10 relates to a ratio of PG/VG/H2O. In preferred embodiments of the present invention, the ratio of PG/VG is more in favour of the PG. That is, in exemplary embodiments the ratio of PG/VG maybe at least 60/40, preferably at least 65/30 and more preferably at least 70/30, and/or at most 90/ 10, preferably at most 80/20 and most preferably at most 70/30. It has been shown that high PG/VG ratios make it possible to provide much more nicotine to the user without additional negative impacts. In addition to the above, in some embodiments, flavouring components may also be added to the aerosol liquid. The aerosol liquids of the present invention are divided into three segments: the tobacco segment, the menthol segment and the fruit segment. Each of the segments represents the dominating flavour of the aerosol liquid. For example, an aerosol liquid of the menthol segment may also have a strawberry taste; as long as the menthol perception is the dominant flavour/perception, it is classified as part of the menthol segment.
The aerosol liquid may also comprise at least one acid, preferably an organic acid. The acid in the aerosol liquid may be any acid from the group of benzoic acid, lactic acid, tartaric acid, sorbic acid, malonic acid, gluconic acid, linoleic acid, saccharic acid, fumaric acid or any combination thereof.
In one example, the aerosol liquid may comprise a combination of benzoic acid, lactic acid, and tartaric acid.
The above acids are known to enhance the fruit or sweet flavour of the liquid. For example, citric acid may be used to enhance the fruit flavour, whereas acids such as saccharic acid or gluconic and/ or malonic acid may enhance both the fruit and the sweet flavour.
However, even though the above acids reduce the negative effect of the nicotine, it has been shown that adding too much of the acids reduces the flavour intensity and in particular the sensational impact of the nicotine. Therefore, it is preferred to keep the total amount of the acids at a sufficiently low level. Exemplary acid-to-nicotine ratios could be anything between o.i:i and 2:1. In some preferred embodiments the acid-to- nicotine molar ratio is 0.1:1, 0.2:1, 0.4:1 or 1:1. Such ratios maybe changing depending on other additives, such as the flavouring components.
Through additives such as the above acids it is further possible to change the pH value of the aerosol liquid. However, other additives that can change the pH value can also be added. It has been shown that the negative effects of high amounts of nicotine are reduced at pH values between 4 and 10. In fact, it has shown that a pH range of 5.5 to 8 provides a particularly pleasant flavour perception and taste satisfaction.
In the above sections, the liquid formulation and in particular the individual properties of the additives have been described. However, the inventors also found that regulating the aerosol collected mass, ACM, can have a positive influence on the sensational IO experience of a user. The ACM conveys similar information as the total particulate matter, TPM, which is commonly used in the context of conventional cigarettes. That is, the TPM relates to the total mass of particles transported in a certain volume of smoke generated by a certain number of conventional cigarettes, whereas for an aerosol generation device the ACM relates to the mass of particles transported in a volume of aerosol generated by a certain number of puffs at the aerosol generation device, such as an e-cigarette or vaporizer.
Currently there are no standardized ISO tests for determining the ACM after a certain number of puffs of an aerosol generation device. To be able to provide similar information as the ISO 4387:2019 (“Cigarettes - Determination of total and nicotine- free dry particulate matter using a routine analytical machine”) for the ACM, a combination of 180:4387:2019 and ISO 20768:2018 was conducted to provide comparable information for an aerosol.
The standard conditions for a routine analytical machine for e-cigarette aerosol for collecting the aerosol mass (ACM) are defined in ISO 20768:2018 (similar to the Coresta Recommended Method No. 81). ISO 20768:2018 defines a routine analytical machine for collecting aerosol from aerosol generating devices. The ACM represents the mass of aerosol collected in an aerosol trapping system when operating a vapor product with the routine analytical vaping machine according to ISO 20768:2018 after a defined number of puffs. The general definitions and conditions are defined in ISO 20768:2018.
Controlling the ACM allows to further increase the overall amount of nicotine in the aerosol liquid without triggering irritations in the nose/throat area. In preferred embodiments, the ACM is at least 85 mg/25 puffs. In further embodiments the ACM is at least 90 mg/25 puffs, preferably at least 100 mg/25 puffs, more preferably at least 110 mg/25 puffs, more preferably at least 115 mg/25 puffs, more preferably at least 125 mg/25 puffs, even more preferably at least 130 mg/25 puffs, and most preferably at least 137 mg/25 puffs, and/or at most 22omg/25 puffs, preferably at most 160 mg/25 puffs particularly at most 140 mg/25 puffs and most preferably at most 137 mg/25 puffs.
In ISO 20768:2018, the pressure drop of a suction mechanism is, the puff duration, puff volume and puff frequency are specified, as well as the puff profile. The puff profile indicates the flow rate measured over the time span of the puffs and shall be of a rectangular shape. That is, the puff profile shows a quick increase in flow rate to a maximum value, which is held for a certain time until the flow rate quickly decreases to a minimum value. The maximum flow rate shall be 18,3 ml/s ± 1.8 ml/s, the total duration of a puff shall be 3 s ± 0,1 s, the puff frequency shall be one puff every 30 s ± 0,5 s, i.e., 2 puffs per minute and the puff volume shall be 55 ml ± 0,6 ml. Also, the device must be fully charged before the measurement to assure the same initial conditions for all the tested devices.
In ISO 20768:2018 it is defined that the ambient conditions of the test environment shall not change considerably during the test. That is, the relative humidity may only change by ± 5% and the temperature by ± 2 °C.
The requirements for the suction machine that performs the puffs are also specified. That is, the machine shall include means to draw a fixed volume of air through the e- cigarette to produce a rectangular shaped profile according to the specification above.
To collect the aerosol drawn from the e-cigarette aerosol traps are specified. That is, an air filter shall be fitted between the suction machine and the e-cigarette. The aerosol traps are specified as comprising an airtight filter holder, and end caps made of a non- hygroscopic material that are able to contain a filter disc of glass fibre material. The glass fibre material has a thickness of 1 mm to 2 mm.
The filter material should retain at least 99% of all particles having a diameter of at least 0.3 pm of a dioctlyl phthalate aerosol with a linear air velocity of 140 mm/s. Wherein the pressure drop of the filter assembly shall not exceed 900 Pa at this air velocity.
With such characteristics, the filter assembly shall be capable of quantitatively retaining the aerosol produced by the e-cigarette without loss. Furthermore, the filter assembly shall be chosen such that the pressure drop of the assembly does not exceed 250 Pa, when measured after the process of collecting the aerosol.
Similar to how the TPM is determined in ISO: 4387:2019, the aerosol collected mass (ACM) is measured gravimetrically (namely: weighted on the scale) as a first assessment. This means, the total number of puffs taken by an analytical machine according to ISO 20768:2018 are recorded and the weight increase of the smoke trap after smoking a certain number of puffs is measured.
The ACM may then be determined according to the formula:
Figure imgf000014_0001
where p is the number of puffs performed m is the mass of the filter assembly after performing p puffs m0 is the mass of the filter assembly before performing any puffs.
For example, an ACM value of 137 means that the mass of the filter assembly has increased by 137 mg after 25 puffs. Which means, that the total mass of the aerosol that is generated within 25 puffs is 137 mg.
The number of puffs has been chosen as 25 (this is not specified in the standard) which is a good compromise between having enough aerosol collected and having not too much mass on the filter to create an air breakthrough (which causes losses).
To control the amount of ACM in the aerosol formed by heating the aerosol liquid, in one embodiment, the aerosol generating device comprises means that allow the control of the ACM to be effectuated. For example, the ACM can be controlled using the controlling means. That is, the ACM may be controlled by controlling the power supplied to the heater of the aerosol generating device. For example, if more power is provided to the heater, which increases the temperature of the heater, the ACM value of the aerosol formed by heating the aerosol liquid increases. Similarly, if less power is provided to the heater, which decreases the temperature of the heater, the ACM value of the aerosol formed by heating the aerosol liquid decreases.
As described above, the aerosol generating device may comprise a determination means for determining the characteristics of the aerosol, such as the ACM. For example, if the determination means comprises a temperature sensor, the ACM may be determined based on the temperature. To do so, the ACM values of individual aerosol liquids may be (pre-) determined in a laboratory at various heater temperatures, using any of the methods described herein (such as ISO 20768:2018 etc.).
When the aerosol generating device is used, the temperature of the heater may then be measured using the temperature sensor. Based on the determined temperature, the corresponding ACM value obtained during the laboratory measurements is determined and considered as the current ACM of the generated aerosol. The controller and/or the determination means may then determine whether the determined ACM value is desired or not. If it is determined that the determined ACM value is not desired, the controlling means may change the power provided to the heater and thereby change the temperature of the heater and the ACM of the generated aerosol. To increase the reliability of the ACM determination in the aerosol generating device, it is preferred to perform the laboratory analysis using a variety of aerosol generating devices and determine the respective ACM values of the respective aerosol generating devices at corresponding temperatures. Even though controlling/ determining the ACM is only described in detail with respect to measuring the temperature, other approaches and determination means are also possible.
In the following, exemplary aerosol liquid compositions with high nicotine amounts will be discussed. That is, the characteristics of various aerosol liquids with 18 mg/ml have been assessed and compared with one another. While the aerosol liquids have similar ingredients, the PG/VG ratio of the respective aerosol liquids vary. As indicated in tables la to ic, four different PG/VG ratios are compared with one another: 30/70, 40/60, 50/50 and 70/30, wherein the aerosol liquids of table la provide a tobacco taste, the aerosol liquids of table ib provide a menthol perception and the aerosol liquids of table ic provide a fruit and sweet taste.
Additionally, for each PG/VG ratio, different ACM values have been used. That is, each of the aerosol liquids have been consumed with an ACM of 75, 110 and 137 and compared with regards to the perceived vapour density, flavour intensity/ sweet taste and amount of irritation/dryness/off-feeling.
The results shown in table la indicate that the amount of aerosol vapour increases with both the PG/VG ratio and the ACM. That is with a constant ACM of 75, the vapour density increases from “lowest” to “mid” for increasing PG/VG ratios. At a constant ACM of 110 the vapour densities increase from “low-mid” to “mid-high” for increasing PG/VG ratios and for a constant ACM of 137 the vapour density increases from “mid” to “high” for increasing PG/VG ratios. Similarly, with a constant PG/VG ratio, the vapour density increases with an increase in ACM. For example, at a PG/VG ratio of 30, the vapour density increases from “lowest” to “mid” with increasing ACM values and at a PG/VG ratio of 80/30 the vapour density increases from “mid” to “high” for increasing ACM values. Table la :
Figure imgf000016_0001
A similar observation was made for the flavour intensity/ sweet taste. That is, the highest flavour intensity for a tobacco flavoured aerosol liquid were experienced at high ACM and high PG/VG ratio, whereas the lowest flavour intensities were experienced at low PG/VG ratios and low ACM values. For the irritation/dryness/off-feel the observation was also in favour of high ACM. It was noticed that the irritation experienced by a user was the lowest for low PG/VG ratio and high ACM. This is not surprising as high PG is known to increase irritation. However, it was also shown, that high PG/VG ratios are still not drastically increasing the irritation/dryness perception when the ACM is also kept at a high level.
For the tobacco flavoured aerosol liquids is could be shown that a combination of high ACM and high PG/VG ratio provide surprisingly well flavour/vapour density/irritation perception to a user. In fact, the perceived flavour intensity and vapour density was the highest for a PG/VG ratio of 70/30 and an ACM value of 137, while the total irritation was kept at a medium range which is acceptable for such a significant increase in vapour density/ flavour intensity/ sweet taste.
Table ib relates to the same test performed for menthol perception aerosol liquids. The results are rather similar, when compared to the tobacco flavoured aerosol liquid. That is, the vapour density increases with the PG/VG ratio and increases with the ACM. Similarly, the flavour intensity/ sweet taste and the cooling experience from the menthol increases with an increase in ACM, and with an increase in PG/VG ratio. Furthermore, the irritation/dryness experience by a user does not exceed a medium level and is tolerable for such a significant increase in vapour density and flavour intensity/ sweet taste/cooling perception. Optimal results with an acceptable amount of irritation were achieved with an ACM of 137 and a PG/VG ratio of 70/30.
Table ib:
Figure imgf000018_0001
In table ic, the results of the user perception experiment are shown for a fruit and/or sweet taste aerosol liquid. For the fruit and/or sweet taste aerosol liquids the vapour density increases with an increase in PG/VG ratio, and simultaneously increases with an increase in ACM. Similarly, the flavour intensity/ sweet taste increases with the ACM and simultaneously increases with an increasing PG/VG ratio. These results are like the other two aerosol liquid flavours (tobacco flavour and menthol flavour). However, for the fruit and/or sweet taste aerosol liquids it has been shown that the irritation/dryness is not only constant for high PG/VG values, but even decreases with increasing ACM values. For example, as shown in table ic, for a PG/VG ratio of 70/30, the irritation/dryness perception decreases for increasing ACM values. That is, an ACM value of 75 results in “high” irritation/dryness perception, whereas an ACM value of no triggers a “mid-high” irritation/dryness perception and an ACM value of 137 triggers only “medium” irritation/dryness perception. Therefore, for fruit and/or sweet flavoured aerosol liquids high ACM values and high PG/VG ratios provide surprisingly beneficial aerosol characteristics for a consumer. In particular, a PG/VG ratio of 70/30 and an ACM value of 137 shows the best results for flavour intensity and vapour density.
Table ic:
Figure imgf000019_0001
With the above it could be shown that an aerosol liquid with high ACM and high PG/VG ratios provide a surprisingly good smoking experience for the user. That is, the negative sensations of high nicotine seem to be mitigated or at least kept at a constantmedium level, while the flavour intensity and vapour density greatly increase. In fact, the overall sensory profile of an i8mg/ ml nicotine aerosol liquid seems to be optimal with an ACM value of 137 and a PG/VG ratio of 70/30 for tobacco/fruit and/or sweet flavoured/ menthol perception tobaccos.
The above results were acquired by using an 18 mg/ ml aerosol liquid formulation. In further embodiments shown in Figs, la to ic, a formulation with varying nicotine, ACM and PG/VG ratios are compared with one another. Again, components of the aerosol that tend to have an impact on the properties of the aerosol liquid, besides flavour components and the components mentioned in Figs, la to ic, were not changed throughout the experiments.
Figures la to ic show plots of the interaction profiles. That is, the amount of perceived discomfort, such as irritation/dryness with respect to the three parameters: amount of nicotine, the ratio of PG/VG and the ACM value. Each of the figures la to ic show a 3x3 plot, wherein each column resembles one changing parameter, and each row resembles two constant values of the respective parameter. Therefore, the 3x3 plot shows the interaction profile of perceived irritation of a user if one isolated component changes. That is, in figures la to ic, column 1 shows the impact on the perceived irritation when only the amount of nicotine is changed, wherein column 2 shows the results of only changing the PG/VG ratio and column 3 shows the respective perceived irritation if only the ACM is changed.
The rows 2 of each of the 3x3 plots show the respective results for a constant component in view of the changing other components. For example, row 1 of figures la to ic show the graphs of an aerosol liquid with of o mg/ ml and a liquid with 12 mg/ ml of nicotine in accordance with changing the PG/VG ratio (row 1, column 2) and the ACM value (row 1, column 3). Row 2 of Figures la to ic shows graphs of a constant PG/VG ratio of 85 and a constant PG/VG ratio of 50 in accordance with changing nicotine amounts (row 2, column 1) and changing ACM (row 2, column 3) and row 3 shows the graphs for a constant PTM of 85 and a constant ACM of 137 in accordance with changing amounts of nicotine (row 3, column 1) and different ratios of PG/VG (rows, column 2). The graphs are plotted with regards to the perceived discomfort of a user. The perceived discomfort is normalized to a range of -0,75 to 1,25, wherein - 0,75 indicates the minimum perceived discomfort (irritation/dryness/off-feel) and 1,25 indicates the maximum perceived discomfort of a user.
In the above example, column 1 of the plot of Fig. la, shows that for tobacco flavoured aerosol liquids the discomfort increases with an increase in both nicotine and PG/VG ratio (column 1, row 2) and is somewhat similar for varying ACM values (column 1, row 3). Column 2 of Fig. la indicates that for high nicotine levels, the irritation slightly increases with an increase of the PG/VG ratio (column 2, row 1) and decreases for high ACM values (column 2, row 3). Column 3, row 2 of Fig. la indicates that an increase in ACM results in a decrease in irritation for high PG/VG ratios and a slight increase for low PG/VG ratios, such that at an ACM of 137, high PG/VG ratios and low PG/VG ratios are perceived similarly, from a perceived irritation point of view (column, 3, row 2). Column 3, row 1 of Fig. la indicates that the perceived irritation decreases for nicotine free aerosol liquids and only slightly increases for high nicotine liquids.
In summary, Fig. la indicates that the negative perception of nicotine increases if only the PG/VG ratio increases. Furthermore, it indicates that the irritation caused by high PG/VG ratios decreases with an increase of ACM. From this, it can be concluded that even if increasing only the PG/VG ratio could have positive benefits on vapour density/ flavour intensity, the amount of irritation might also increase. Thus, only if parallel to an increase of the PG/VG ratio the ACM increases can the positive effects be achieved while the irritation is at least kept at a constant amount. This observation confirms the results shown in table la.
Figure lb shows the interaction profile for aerosol liquids in the menthol segment. The plots of column 1 of Fig. lb indicate that the perceived discomfort for increasing nicotine amounts is similar for high and low PG/VG ratios and high and low ACM values. Furthermore, the plots of column 2 of Fig. lb indicate that the irritation for high nicotine liquids decreases with an increase of PG/VG (column 2, rowi) and slightly increases for high ACM values, whereas the irritation reduces with increasing PG/VG values for low ACM values (columns 2, rows). Additionally, column 3 indicates that the perceived negative effect of either nicotine or high PG/VG reduces with an increase of ACM.
The above confirms that the overall negative sensation is reduced with an increase of the ACM value. In fact, the minimum negative perception is achieved for ACM values of 137, which confirms the results shown in table lb. Furthermore, high PG/VG ratios, that provides excellent flavour intensity/ vapour density, only slightly increase the perceived discomfort, when compared to low PG/VG values and appear to not have an impact on the discomfort caused by high nicotine values (cf. Fig. lb, column 2, row2). Therefore, this test further confirms that high PG/VG ratios combined with high ACM values provide good properties whilst the negative effect of high PG/Vg is surprisingly significantly reduced.
In the fruit segment, as displayed in Fig. ic, the above observations are confirmed. In fact, for the fruit segment the above effects are even more significant. That is, column i of Fig. ic shows that the discomfort experienced by a user due to high nicotine amounts is independent from the PG/VG ratio (column 1, row 2). However, it seems that high ACM values drastically reduce the irritation, when compared to low ACM values (column 1, row 3). Column 2 of Fig. ic shows that when only the PG/VG is changed amount of irritation was perceived for a PG/VG ratio of around 70/30 and increases from there for lower and higher PG/VG ratios. This observation was made for high and low nicotine amounts (column 2, row 1) and high and low ACM values (column 2, row 3). In addition, when only changing the amount of ACM, a decrease in irritation was noticed for high amounts of nicotine (column 3, row 1) and a similar amount of irritation for high and low PG/VG ratios (column 3, row 2).
Consequently, Fig. ic shows that for the fruit segment, the optimal PG/VG ratio appears to be 70/30. In addition, increasing amounts of ACM provide a strong positive effect for high nicotine formulations.
In summary, the test results of Figs, la to ic show that in the tobacco segment the additional irritation caused by high PG/VG ratios at high nicotine levels can be mitigated through high ACM values. Therefore, it is possible to provide high nicotine tobacco flavoured aerosol liquids without the negative sensations caused by the nicotine if both the ACM and the PG/VG ratio are high.
For the menthol segment, the results show that the PG/VG seems to have no isolated impact on the negative perceived sensation of increasing amounts of nicotine.
However, since high ACM values reduce the negative impact of the nicotine, the combination of high PG/VG ratio and high ACM seems to reduce the overall negative effects, whilst maintaining the beneficial effects of an increase in vapour density/ flavour intensity caused by the high PG/VG ratio and the high ACM. For the fruit segment and exceptional positive effect was observed for a PG/VG ratio in the area of 70/30. That is, the closer the PG/VG ratio is to a ratio of 70/30, the weaker is a perceived negative impact of the nicotine. This appears to be valid for low amounts of nicotine as well as high amounts of nicotine. In fact, in the fruit segment high ACM values also decrease the negative impact of high amounts of nicotine, such that a PG/VG of 70/30 and an ACM of 137 provides exceptional positive results for this segment.
From the above, it becomes apparent that one preferred embodiment of the invention is to use a PG/VG ratio of 70/30 and an ACM value of 137. In fact, this combination shows the best overall results and in particular the best results in the fruit segment. However, it also shows that in other embodiments, and in particular in such embodiments that are in the tobacco segment or the menthol segment, other PG/VG ratios and ACM values could be preferred.
For example, in one embodiment of an aerosol liquid in the menthol segment, a PG/VG ratio of 85/ 15 could be better suited for some applications, as indicated in Fig. ib.
It is apparent for the skilled person, that the combinations and ratios provided by the above description maybe changed as desired. For example, in some embodiments if it is required by law, it may even be desired to maintain low amounts of the negative impact of the nicotine. Since the above invention provides a method to reduce the negative effects of high amounts of nicotine, tailoring the aerosol liquid to provide some negative impact does not contradict with the essence of the invention. In fact, some users desire a strong “throat hit” when using an aerosol generation device. Therefore, when maintaining some of the negative effects of the nicotine means that the overall amount of nicotine, PG, VG, flavour components etc. may be increased even further, such that the positive sensational experience of a user caused by these components may further increase.

Claims

Claims
1. A method of delivering an aerosol from an aerosol liquid heated in an aerosol generating device comprising an electrical heater, wherein the aerosol liquid comprises: at least 55 wt. % of propylene glycol, PG; glycerol; and at least 3 mg/ ml of nicotine; and wherein the delivery of the aerosol is controlled by the device such that the aerosol collected mass, ACM, is at least 85 mg/25 puffs when the puffs are performed and the aerosol is collected by an analytical machine according to ISO 20768:2018.
2. The method according to the preceding claim, wherein the ratio between PG and glycerol is at least 60:40, preferably at least 65:35 and more preferably at least 70:30; and/or at most 90:10, preferably at most 80:20 and most preferably at most 70:30.
3. The method according to any one of the preceding claims, wherein the delivery of the aerosol is controlled by the device such that the ACM is at least 90 mg/25 puffs, preferably at least 100 mg/25 puffs, more preferably at least 110 mg/25 puffs, more preferably at least 115 mg/25 puffs, more preferably at least 125 mg/ 25 puffs, even more preferably at least 130 mg/ 25 puffs most preferably at least 137 mg/25 puffs; and/or at most 220 mg/25 puffs, preferably at most 180 mg/25 puffs, more preferably at most 160 mg/25 puffs, particularly at most 140 mg/25 puffs and is most preferably at most 137 mg/25 puffs.
4. The method according to any one of the preceding claims, wherein the aerosol liquid comprises at least 60 wt. % of PG, preferably at least 65 wt. % of PG, and/or at most 90 wt. % of PG, preferably at most 80 wt. % of PG.
5. The method according to any one of the preceding claims, wherein the aerosol liquid comprises at least 6 mg/ml of nicotine, preferably at least 8 mg/ml of nicotine and more preferably at least 12 mg/ml of nicotine; and/or at most 59 mg/ml of nicotine, preferably at most 40 mg/ml of nicotine, more preferably at most 20 mg/ml of nicotine and most preferably at most 18 mg/ml.
6. The method according to any one of the preceding claims, wherein the aerosol liquid further comprises a flavour component in an amount between 1 and 25 wt. % of the aerosol liquid, preferably between 2 and 20 wt. %.
7. The method according to any one of the preceding claims, wherein the aerosol liquid comprises at least one acid, preferably an organic acid, more preferably one or more of benzoic acid, lactic acid, tartaric acid, malic acid, most preferably a combination of benzoic acid, lactic acid and tartaric acid.
8. The method according to the preceding claim, wherein the acid-to- nicotine molar ratio is at least 0.1:1 preferably at least 0.2:1, and/or at most 2:1, preferably at most 1:1.
9. The method according to any one of the preceding claims, wherein the pH of the aerosol liquid is between 4 and 10, preferably between 5.5 and 8.
10. The method according to any one of the preceding claims, wherein the aerosol generating device is an e-cigarette.
11. The method according to any one of the preceding claims, wherein the ACM is determined gravimetrically.
12. The method according to any one of the preceding claims, wherein the ACM is determined according to the formular: m ACM = —
P wherein m is the weight of the aerosol mass collected by the analytical machine and p is the total amounts of puffs.
13. The method according to any one of the preceding claims, wherein the amount of the ACM is determined according to the test method specified in ISO 4387:2019. 14- An aerosol generating device for delivering an aerosol from an aerosol liquid, comprising an electrical heater and being configured to carry out the method according to any one of claims 1 to 13.
PCT/EP2023/054818 2022-02-28 2023-02-27 Provision of high nicotine aerosol WO2023161465A1 (en)

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Citations (6)

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US9215895B2 (en) 2013-05-06 2015-12-22 Pax Labs, Inc. Nicotine salt formulations for aerosol devices and methods thereof
US20170215470A1 (en) * 2014-07-10 2017-08-03 Laboratoires Ceres Use of a composition containing a long-chain polyol as a base for e-liquids
CN110367592A (en) * 2013-07-19 2019-10-25 奥驰亚客户服务有限责任公司 The liquid aerosol formulations of electrical smoking utensil
RU2707892C2 (en) * 2015-09-01 2019-12-02 Аир Лтд Electronic evaporator system
EP3639813A1 (en) 2014-05-21 2020-04-22 McNeil AB A liquid formulation comprising nicotine for aerosol administration

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9215895B2 (en) 2013-05-06 2015-12-22 Pax Labs, Inc. Nicotine salt formulations for aerosol devices and methods thereof
CN110367592A (en) * 2013-07-19 2019-10-25 奥驰亚客户服务有限责任公司 The liquid aerosol formulations of electrical smoking utensil
US20150313275A1 (en) * 2014-04-30 2015-11-05 Altria Client Services, Inc. Liquid aerosol formulation of an electronic smoking article
EP3639813A1 (en) 2014-05-21 2020-04-22 McNeil AB A liquid formulation comprising nicotine for aerosol administration
US20170215470A1 (en) * 2014-07-10 2017-08-03 Laboratoires Ceres Use of a composition containing a long-chain polyol as a base for e-liquids
RU2707892C2 (en) * 2015-09-01 2019-12-02 Аир Лтд Electronic evaporator system

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