WO2015129679A1 - 香喫味成分の抽出方法及び嗜好品の構成要素の製造方法 - Google Patents
香喫味成分の抽出方法及び嗜好品の構成要素の製造方法 Download PDFInfo
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- WO2015129679A1 WO2015129679A1 PCT/JP2015/055208 JP2015055208W WO2015129679A1 WO 2015129679 A1 WO2015129679 A1 WO 2015129679A1 JP 2015055208 W JP2015055208 W JP 2015055208W WO 2015129679 A1 WO2015129679 A1 WO 2015129679A1
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
- A24B15/167—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes in liquid or vaporisable form, e.g. liquid compositions for electronic cigarettes
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/241—Extraction of specific substances
- A24B15/243—Nicotine
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/287—Treatment of tobacco products or tobacco substitutes by chemical substances by inorganic substances only
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
- A24D3/14—Use of materials for tobacco smoke filters of organic materials as additive
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/26—Use of organic solvents for extraction
Definitions
- the present invention relates to a method for extracting flavor components and a method for producing components of luxury products.
- a flavor component for example, an alkaloid containing a nicotine component
- a tobacco raw material for example, a tobacco raw material
- the extracted flavor component is supported on a flavor source substrate.
- a technique related to a method for extracting a flavor component for example, a method for extracting a flavor component (hereinafter referred to as a first conventional technology), for example, a method for removing a flavor component from a tobacco raw material using ammonia gas is known (for example, a patent). Reference 1).
- a supercritical extraction method using an extraction solvent and a trapping solvent is known as a technique related to a method for extracting a flavor component (hereinafter, second conventional technique) (for example, Patent Document 2).
- a first feature is a method for extracting a flavor ingredient from a tobacco raw material, which is a process A for heating a tobacco raw material that has been subjected to alkali treatment, and the second condition after the first condition is satisfied.
- a step B in which the release component released into the gas phase in the step A is brought into contact with a normal temperature collection solvent until any timing until the condition is satisfied, and the content of sugars contained in the tobacco raw material In the dry state, when the total weight of the tobacco raw material is 100% by weight, it is 9.0% by weight or less, and the first condition is a time axis that has elapsed since the start of the step A.
- the process A The time elapsed from the start is a condition for reaching the start timing of the stable section, and the second condition is included in the tobacco raw material when the weight of the tobacco raw material is 100% by weight in a dry state.
- the gist is that the condition is such that the remaining amount of the nicotine component, which is an indicator of the flavor component, decreases until it reaches 0.3% by weight.
- the second feature is that, in the first feature, the second condition is that when the weight of the tobacco raw material is 100% by weight in a dry state, the residual amount of the nicotine component contained in the tobacco raw material is 0.
- the main point is that the conditions are reduced until reaching 4% by weight.
- the second condition is that when the weight of the tobacco raw material is 100% by weight in a dry state, the residual amount of the nicotine component contained in the tobacco raw material is 0. The main point is that the conditions are reduced until reaching 6% by weight.
- the second condition is that when the weight of the tobacco raw material is 100% by weight in a dry state, the residual amount of the nicotine component contained in the tobacco raw material is 0.
- the gist is that the condition is reduced until it reaches 7% by weight.
- the fifth feature is summarized in that in any one of the first to fourth features, the tobacco raw material is subjected to a hydration treatment in the step A.
- the sixth feature is summarized as any one of the first to fifth features, wherein the tobacco raw material is a tobacco raw material of Burley species.
- a seventh feature is a method for manufacturing a component of a luxury product, which includes a process A for heating a tobacco raw material that has been subjected to an alkali treatment, and from when the first condition is satisfied until the second condition is satisfied. Until that timing, the release component released into the gas phase in the step A is brought into contact with a normal temperature collection solvent to obtain a collection solution, and the step of adding the collection solution to the constituent elements C, and the total content of sugars contained in the tobacco raw material is 9.0% by weight or less when the total weight of the tobacco raw material is 100% by weight in the dry state.
- the condition is that after the pH of the collection solution containing the collection solvent and the release component has decreased from the maximum value by 0.2 or more on the time axis that has elapsed since the start of the step A, the collection solution
- the amount of fluctuation in pH is within the specified range.
- the time elapsed since the start of the step A is a condition for reaching the start timing of the stable section
- the second condition is that the weight of the tobacco raw material is 100% by weight in a dry state.
- the gist is that the remaining amount of the nicotine component contained in the tobacco raw material is reduced until it reaches 0.3% by weight.
- FIG. 1 is a diagram illustrating an example of an extraction device according to the first embodiment.
- FIG. 2 is a diagram illustrating an example of the extraction device according to the first embodiment.
- FIG. 3 is a diagram for explaining an application example of the flavor component.
- FIG. 4 is a flowchart showing the extraction method according to the first embodiment.
- FIG. 5 is a diagram for explaining the first experiment.
- FIG. 6 is a diagram for explaining the first experiment.
- FIG. 7 is a diagram for explaining the first experiment.
- FIG. 8 is a diagram for explaining the second experiment.
- FIG. 9 is a diagram for explaining the second experiment.
- FIG. 10 is a diagram for explaining the second experiment.
- FIG. 11 is a diagram for explaining the second experiment.
- FIG. 12 is a diagram for explaining the third experiment.
- FIG. 13 is a diagram for explaining the third experiment.
- FIG. 14 is a diagram for explaining the fourth experiment.
- FIG. 15 is a diagram for explaining the fourth experiment.
- the extraction method of the flavor component which concerns on embodiment is an extraction method which extracts a flavor component from a tobacco raw material.
- the tobacco raw material subjected to the alkali treatment is heated in the gas phase in the process A until any timing from when the first condition is satisfied until the second condition is satisfied after the process A is heated.
- the total content of sugars contained in the tobacco raw material is 9.0% by weight or less when the total weight of the tobacco raw material is 100% by weight in a dry state.
- the first condition is that after the pH of the collection solution containing the collection solvent and the release component has decreased by 0.2 or more from the maximum value on the time axis that has elapsed since the start of the step A, When there is a stable section where the amount of change in the pH of the collection solution falls within a predetermined range, the time elapsed from the start of the step A is a condition for reaching the start timing of the stable section.
- the second condition is that, in a dry state, when the weight of the tobacco raw material is 100% by weight, the residual amount of the nicotine component that is an indicator of the flavor ingredient contained in the tobacco raw material is 0.3% by weight. It is a condition that decreases until it is reached.
- the step B of bringing the release component into contact with the collection solvent continues at least until the first condition is satisfied.
- ammonium ions (NH 4 + ) contained in the release component are sufficiently removed from the collection solution.
- volatile contaminants (acetaldehyde, pyridine, etc.) other than ammonium ions are also removed from the collection solution.
- the step B in which the released component is brought into contact with the collection solvent is completed until at least the second condition is satisfied. Thereby, the increase in the content of TSNA contained in the collection solution is suppressed by ending Step B before the release amount of tobacco-specific nitrosamine (TSNA: Tobacco Specific Nitrosamines) increases.
- TSNA tobacco-specific nitrosamine
- the flavor component can be sufficiently extracted by suppressing the contamination of ammonium ions (NH 4 + ) and TSNA and the like by simple treatments such as Step A and Step B. That is, a savory component can be extracted with a simple device.
- the nicotine component is an example of a flavor component that contributes to tobacco flavor, and is used as an indicator of the flavor component in the embodiment.
- FIGS. 1 and 2 are diagrams illustrating an example of an extraction device according to the first embodiment.
- the alkali treatment apparatus 10 includes a container 11 and a sprayer 12.
- the container 11 accommodates the tobacco raw material 50.
- the container 11 is comprised by the member (for example, SUS; Steel Used Stainless) which has heat resistance and pressure resistance, for example.
- the container 11 preferably constitutes a sealed space. “Enclosed space” is a state in which solid foreign substances are prevented from being mixed during normal handling (transportation, storage, etc.). Thereby, volatilization of the flavor component contained in the tobacco raw material 50 to the outside of the container 11 is suppressed.
- the sprayer 12 applies an alkaline substance to the tobacco raw material 50.
- the alkaline substance for example, a basic substance such as an aqueous potassium carbonate solution is preferably used.
- the sprayer 12 applies an alkaline substance to the tobacco raw material 50 until the pH of the tobacco raw material 50 becomes 8.0 or more. More preferably, the sprayer 12 preferably applies an alkaline substance to the tobacco raw material 50 until the pH of the tobacco raw material 50 is in the range of 8.9 to 9.7. Further, in order to efficiently release flavor components from the tobacco raw material 50 into the gas phase, the moisture content of the tobacco raw material 50 after spraying the alkaline substance is preferably 10% by weight or more, and more preferably 30% by weight or more. More preferably. Although the upper limit of the moisture content of the tobacco raw material 50 is not specifically limited, For example, in order to heat the tobacco raw material 50 efficiently, it is preferable to set it as 50 weight% or less.
- the total content of saccharides contained in the tobacco raw material 50 is 9.0% by weight or less when the total weight of the tobacco raw material 50 is 100% by weight in the dry state.
- the saccharide contained in the tobacco raw material 50 is sucrose (sucrose), fructose, glucose, maltose, inositol.
- the initial content of the flavor component (here, nicotine component) contained in the tobacco raw material 50 is 2.0% by weight or more when the total weight of the tobacco raw material 50 is 100% by weight in the dry state. Preferably there is. More preferably, the initial content of the flavor component (here, nicotine component) is preferably 4.0% by weight or more.
- the tobacco raw material 50 for example, a tobacco genus raw material such as Nicotiana tabacum or Nicotiana rustica can be used.
- Nicotiana tabacam for example, varieties such as Burley or yellow can be used.
- tobacco raw materials other than Burley species and yellow species may be used.
- the total content of sugars contained in the tobacco raw material 50 is 9.0 weight. It is preferable to use the tobacco raw material 50 which is not more than%. More preferably, the total content of sugars contained in the tobacco raw material 50 is preferably 1.0% by weight or less. More preferably, the total content of sugars contained in the tobacco raw material 50 is preferably 0.7% by weight or less.
- the tobacco raw material 50 may be composed of tobacco raw materials in chopped or granular form.
- the particle size of the step or powder is preferably 0.5 mm to 1.18 mm.
- the collection device 20 includes a container 21, a pipe 22, a discharge portion 23, and a pipe 24.
- the container 21 contains the collection solvent 70.
- the container 21 is made of glass, for example.
- the container 21 preferably constitutes a sealed space. “Enclosed space” is a state in which solid foreign substances are prevented from being mixed during normal handling (transportation, storage, etc.).
- the temperature of the collection solvent 70 is, for example, room temperature.
- the lower limit of the normal temperature is, for example, a temperature at which the collection solvent 70 does not solidify, preferably 10 ° C.
- the upper limit of normal temperature is 40 degrees C or less, for example.
- An arbitrary acid such as malic acid or citric acid may be added to the collection solvent 70 in order to prevent re-volatilization of the flavor component captured by the collection solvent 70.
- a component or substance such as an aqueous citric acid solution may be added to the collection solvent 70. That is, the collection solvent 70 may be composed of a plurality of types of components or substances.
- the initial pH of the collection solvent 70 is preferably lower than the pH of the tobacco raw material 50 after the alkali treatment.
- the pipe 22 guides the released component 61 released from the tobacco raw material 50 into the gas phase by heating the tobacco raw material 50 to the collection solvent 70.
- the release component 61 includes at least a nicotine component that is an index of the flavor component. Since the tobacco raw material 50 has been subjected to alkali treatment, the release component 61 may contain ammonium ions depending on the time (treatment time) that has elapsed since the start of the step of collecting the flavor and taste components. The release component 61 may contain TSNA depending on the time (processing time) that has elapsed since the start of the collection process.
- the discharge part 23 is provided at the tip of the pipe 22 and is immersed in the collection solvent 70.
- the discharge portion 23 has a plurality of openings 23A.
- the release component 61 guided by the pipe 22 is released into the collection solvent 70 as a foam-like release component 62 from the plurality of openings 23A.
- the pipe 24 guides the remaining component 63 not captured by the collection solvent 70 to the outside of the container 21.
- the release component 62 is a component released into the gas phase by heating the tobacco raw material 50, there is a possibility that the temperature of the collection solvent 70 is increased by the release component 62. Therefore, the collection device 20 may have a function of cooling the collection solvent 70 in order to maintain the temperature of the collection solvent 70 at room temperature.
- the collection device 20 may have a Raschig ring in order to increase the contact area of the release component 62 with the collection solvent 70.
- FIG. 3 is a diagram for explaining an application example of the flavor component.
- the flavor component is given to a component of a luxury item (for example, a flavor source of a flavor suction tool).
- the flavor suction device 100 includes a holder 110, a carbon heat source 120, a flavor source 130, and a filter 140.
- the holder 110 is, for example, a paper tube having a cylindrical shape.
- the carbon heat source 120 generates heat for heating the flavor source 130.
- the flavor source 130 is a substance that generates a flavor, and is an example of a flavor source base material to which an alkaloid containing a nicotine component is added.
- the filter 140 suppresses the contamination material from being guided to the inlet side.
- the flavor suction tool 100 has been described as an application example of the flavor component, but the embodiment is not limited thereto.
- the flavor component may be applied to other suction devices such as an electronic cigarette aerosol source (so-called E-ligid).
- a flavor component may be provided to flavor source base materials, such as a gum, a tablet, a film, and a candy.
- FIG. 4 is a flowchart showing the extraction method according to the first embodiment.
- an alkaline substance is applied to the tobacco raw material 50 using the alkali treatment apparatus 10 described above.
- the alkaline substance for example, a basic substance such as an aqueous potassium carbonate solution can be used.
- the total content of saccharides contained in the tobacco raw material 50 is 9.0% by weight or less when the total weight of the tobacco raw material 50 is 100% by weight in the dry state as described above.
- the saccharide contained in the tobacco raw material 50 is fructose, glucose, saccharose, maltose, inositol.
- the initial content of the flavor component (here, nicotine component) contained in the tobacco raw material 50 is 2.0% by weight or more when the total weight of the tobacco raw material 50 is 100% by weight in the dry state. Preferably there is. More preferably, the initial content of the flavor component (here, nicotine component) is preferably 4.0% by weight or more.
- the pH of the tobacco raw material 50 after the alkali treatment is preferably 8.0 or more. More preferably, the pH of the tobacco raw material 50 after the alkali treatment is preferably in the range of 8.9 to 9.7.
- the tobacco raw material 50 may be subjected to a hydration treatment.
- the moisture content of the tobacco raw material 50 before the water treatment is preferably 10% by weight or more, and more preferably 30% by weight or more.
- the upper limit of the moisture content of the tobacco raw material 50 is not specifically limited, For example, in order to heat the tobacco raw material 50 efficiently, it is preferable to set it as 50 weight% or less.
- step S20 the tobacco raw material 50 that has been subjected to the alkali treatment is heated.
- the tobacco raw material 50 can be heated together with the container 11 in a state where the tobacco raw material 50 is accommodated in the container 11 of the alkali treatment apparatus 10.
- the pipe 22 of the collection device 20 is attached to the container 11.
- the heating temperature of the tobacco raw material 50 is in the range of 80 ° C. or more and less than 150 ° C.
- the timing at which a sufficient flavor component is released from the tobacco raw material 50 can be advanced.
- the timing at which TSNA is released from the tobacco raw material 50 can be delayed.
- the tobacco raw material 50 may be subjected to a hydration treatment.
- the moisture content of the tobacco raw material 50 after the hydration treatment is preferably 10% or more and 50% or less.
- the tobacco raw material 50 may be continuously hydrated. The amount of water added is preferably adjusted so that the moisture content of the tobacco raw material 50 is 10% or more and 50% or less.
- step S20 it is preferable to subject the tobacco material 50 to aeration.
- the amount of flavor components contained in the release component 61 released from the tobacco-treated tobacco material 50 into the gas phase can be increased.
- the aeration treatment for example, saturated water vapor at 80 ° C. is brought into contact with the tobacco raw material 50. Since the aeration time in the aeration treatment varies depending on the apparatus for treating the tobacco raw material 50 and the amount of the tobacco raw material 50, it cannot be specified in general. For example, when the tobacco raw material 50 is 500 g, the aeration time is Within 300 minutes.
- the total aeration amount in the aeration treatment also varies depending on the apparatus for treating the tobacco raw material 50 and the amount of the tobacco raw material 50, and thus cannot be generally specified. For example, when the tobacco raw material 50 is 500 g, 10 L / It is about g.
- the air used in the ventilation process may not be saturated water vapor.
- the moisture content of the air used in the aeration treatment does not particularly require humidification of the tobacco raw material 50, for example, so that the moisture contained in the tobacco raw material 50 to which the heat treatment and the aeration treatment are applied falls within a range of less than 50%. May be adjusted.
- the gas used in the aeration process is not limited to air, and may be an inert gas such as nitrogen or argon.
- step S30 using the collection device 20 described above, the release component released into the gas phase in step S20 is set to room temperature until any timing from when the first condition is satisfied until the second condition is satisfied. It is made to contact with the collection solvent 70 of this.
- step S20 and step S30 are shown as separate processes in FIG. 4, but it should be noted that steps S20 and S30 are processes performed in parallel. Note that parallel means that the period in which step S30 is performed overlaps with the period in which step S20 is performed, and step S20 and step S30 do not have to start and end at the same time.
- the pressure in the container 11 of the alkali treatment apparatus 10 is equal to or lower than the normal pressure.
- the upper limit of the pressure in the container 11 of the alkali treatment apparatus 10 is +0.1 MPa or less in terms of gauge pressure.
- the inside of the container 11 of the alkali treatment apparatus 10 may be a reduced pressure atmosphere.
- the collection solvent 70 as described above, for example, glycerin, water, or ethanol can be used.
- the temperature of the collection solvent 70 is room temperature as described above.
- the lower limit of the normal temperature is, for example, a temperature at which the collection solvent 70 does not solidify, preferably 10 ° C.
- the upper limit of normal temperature is 40 degrees C or less, for example.
- the first condition is that after the pH of the collection solution containing the collection solvent 70 and the release component 62 has decreased from the maximum value by 0.2 or more on the time axis that has elapsed since the start of step S20, the collection solution
- the time elapsed after the start of step S20 (hereinafter, processing time) is a condition for reaching the start timing of the stable section.
- the stable section is a section in which the amount of fluctuation in the pH of the collection solution falls within a predetermined range (for example, the average amount of fluctuation per unit time is ⁇ 0.01 / min), and in this section
- the fluctuation range of the pH of the collection solution is a section that falls within a predetermined range (for example, the difference between the pH when the section starts and the pH when the second condition described later is satisfied is ⁇ 0.2).
- the start timing of the stable section is, for example, This is the timing when the pH of the collection solution stops decreasing.
- the pH profile of the collection solution is measured in advance under the same conditions as those in the actual treatment, and the pH of the collection solution is replaced with the treatment time. That is, it is preferable that the first condition is replaced with the processing time. Accordingly, it is not necessary to monitor the amount of fluctuation of the pH of the collection solution in real time, and ammonium ions (NH 4 + ) can be removed from the collection solution by simple control.
- the second condition is that when the weight of the tobacco raw material 50 is 100% by weight in the dry state, the remaining amount of the flavor component (here, the nicotine component) contained in the tobacco raw material 50 reaches 0.3% by weight. It is a condition to decrease to. More preferably, the second condition is that when the weight of the tobacco raw material 50 is 100% by weight in the dry state, the remaining amount of the flavor component (here, the nicotine component) contained in the tobacco raw material 50 is 0.4. It is a condition that decreases until reaching% by weight. More preferably, the second condition is that, in a dry state, when the weight of the tobacco raw material 50 is 100% by weight, the remaining amount of the flavor component (here, the nicotine component) contained in the tobacco raw material 50 is 0.6.
- the second condition is that when the weight of the tobacco raw material 50 is 100% by weight in the dry state, the remaining amount of the flavor component (here, the nicotine component) contained in the tobacco raw material 50 is 0.7. It is a condition that decreases until reaching% by weight.
- the profile of the remaining amount of the flavor component (here, the nicotine component) contained in the tobacco raw material 50 is measured in advance under the same conditions as those in the actual processing, and the remaining amount of the flavor component is determined by the processing. It is preferred that it be replaced by time. That is, it is preferable that the second condition is replaced with the processing time. Thereby, it is not necessary to monitor the remaining amount of the flavor component in real time, and it is possible to suppress an increase in the content of TSNA contained in the collection solution by simple control.
- step S40 in order to increase the concentration of the flavor component contained in the collection solution, the vacuum concentration treatment, the heat concentration treatment or the collection solvent 70 that captures the flavor component (that is, the collection solution) is used. A salting-out treatment is performed.
- vacuum concentration treatment is performed in a sealed space, there is little air contact and there is no need to raise the temperature of the collection solvent 70, so there is little concern about component changes. Accordingly, the use of vacuum concentration increases the types of collection solvent that can be used.
- salting-out treatment it is possible to increase the concentration of the flavor component compared to the vacuum concentration treatment, but since the flavor component is separated into the liquid solvent phase and the aqueous phase, the yield of the flavor component is increased. Is bad. Moreover, since coexistence of a hydrophobic substance (MCT etc.) is assumed to be essential, salting-out may not occur depending on the ratio of the collection solvent, water and flavor components.
- MCT hydrophobic substance
- step S50 the collection solution containing the flavor component is added to the component of the luxury item. That is, in step S50, the flavor component captured by the collection solvent 70 is carried on the flavor source base material (component of the favorite product).
- step S40 and step S50 is not an essential process.
- step S30 which makes a discharge
- ammonium ions (NH 4 + ) contained in the release component are sufficiently removed from the collection solution.
- other volatile impurities specifically, acetaldehyde and pyridine
- step S30 for bringing the released component into contact with the collection solvent 70 ends at least until the second condition is satisfied.
- the increase in the content of TSNA contained in the collection solution is suppressed by terminating S30 before the amount of TSNA released increases.
- step S20 and step S30 it is possible to sufficiently extract the flavor components while suppressing the mixing of ammonium ions (NH 4 + ) and contaminating components such as TSNA. That is, a savory component can be extracted with a simple device.
- ammonium ions NH 4 +
- contaminating components such as TSNA
- the non-volatile component contained in the tobacco raw material 50 is not transferred to the collection solvent, but only the component that volatilizes at about 120 ° C. can be collected in the collection solvent, the component collected by the collection solvent Is effective as an aerosol source for electronic cigarettes.
- This makes it possible to deliver an aerosol containing tobacco flavor to the user while suppressing the increase of volatile impurities such as ammonium ions, acetaldehyde, and pyridine in the electronic cigarette, and further suppresses the burning of the heater that heats the aerosol source. be able to.
- electrocigarette includes a liquid aerosol source and an electric heater for heating and atomizing the aerosol source, and a non-combustion flavor inhaler or aerosol suction for delivering the aerosol to the user.
- aerosol inhaler described in Japanese Patent No. 5196673, aerosol electronic cigarette described in Japanese Patent No. 5385418, etc.
- aerosol suction for delivering the aerosol to the user.
- the flavor component of the tobacco raw material 50 is brought into contact with the flavor component released from the tobacco raw material 50 in step S30.
- the collection solvent namely, collection solution
- the collection solution added to the tobacco raw material residue may be neutralized.
- the tobacco raw material residue containing the flavor component may be neutralized after adding the collection solution to the tobacco raw material residue.
- the amount of flavor component (here, nicotine component) contained in the tobacco raw material after the collection solution is applied back to the tobacco raw material residue in the wrapping treatment is included in the tobacco raw material before releasing the flavor component. It should be noted that the amount is less than or equal to the flavor component (here, the nicotine component).
- the tobacco raw material 50 after releasing the flavor component in step S20 may be washed with a washing solvent before performing the above-described retraction process.
- a washing solvent can be mentioned as a washing
- a pure water and an ultrapure water may be sufficient, and a city water can be mentioned.
- the nicotine content (Nic. Amount) and ammonium ion content (NH 4 + amount) of Sample A to Sample D are as shown in FIG.
- the content of saccharides (fructose, glucose, saccharose, maltose, inositol) of sample A is almost zero (below the detection limit), and the saccharides of sample B (fructose, glucose, saccharose, maltose, inositol)
- the total content is 9.37% by weight
- the total content of saccharides (fructose, glucose, saccharose, maltose, inositol) of sample C is 18.81% by weight
- processing time is the time which passed after starting the heat processing (S20) of a tobacco raw material. You may think that processing time is the time which passed since the collection process (S30) of a flavor component (in the following, nicotine component) was started.
- the gas used in the bubbling process is an atmosphere of about 20 ° C. and about 60% -RH.
- sample B as shown in FIG. 6, in the pH profile of the collection solution, it was confirmed that there was no section in which the pH of the collection solution decreased by 0.2 or more from the maximum value.
- sample C as shown in FIG. 6, in the pH profile of the collection solution, it was confirmed that the pH of the collection solution was intermittently reduced and the above-described stable section was not present.
- the stable section is a section in which the amount of fluctuation in the pH of the collection solution is within a predetermined range (for example, the average amount of fluctuation per unit time is ⁇ 0.01 / min), and
- the fluctuation range of the pH of the collection solution in the section is within a predetermined range (for example, the difference between the pH when the section starts and the pH when the second condition described later is satisfied is ⁇ 0.2). It is a section that fits.
- the burley tobacco material having a low saccharide content in the tobacco material specifically, the total content of saccharides in the tobacco material is 9.0% by weight. It was confirmed that by using the following tobacco raw materials, it was possible to clearly determine the stable pH section indicating that the ammonium ion concentration in the collection solution was sufficiently reduced. In addition, the use of a Burley-type tobacco raw material having a high ammonium ion (NH 4 + ) concentration makes it easy to determine the profile accompanying a decrease in pH.
- the measurement results of the nicotine concentration and nicotine recovery rate in the tobacco raw material of Sample A are as shown in FIG. 8, and the measurement results of the nicotine concentration and nicotine recovery rate in the tobacco raw material of Sample D are as shown in FIG. Moreover, the measurement result of the concentration of TSNA contained in the collection solution of sample A is as shown in FIG. 10, and the measurement result of the concentration of TSNA contained in the collection solution of sample D is as shown in FIG. is there.
- the concentration of nicotine in the tobacco raw material is indicated by weight% when the weight of the tobacco raw material is 100% by weight in the dry state.
- the nicotine recovery rate is shown as a ratio with respect to the initial weight of the nicotine component contained in the tobacco raw material in the dry state.
- the concentration of TSNA contained in the collection solution is shown in wt% when the collection solution is 100 wt%. 8 to 11, the processing time is the time that has elapsed since the start of the tobacco raw material heat treatment (S20). You may think that processing time is the time which passed since the collection processing (S30) of a nicotine component was started.
- NNK N′-Nitrosonoricotine
- NNN N′-Nitrosonatabine
- NAB Nitrosonabasine
- the gas used in the bubbling process is an atmosphere of about 20 ° C. and about 60% -RH.
- the rate of decrease in the remaining amount of the nicotine component contained in the tobacco raw material (that is, The rate at which the nicotine component volatilizes from the tobacco raw material) has decreased, and it has been confirmed that an increase in the recovery rate of the nicotine component cannot be expected.
- the NAB in the collection solution gradually increased when the treatment time exceeded the timing at which the nicotine concentration in the tobacco raw material reached 0.4% by weight (180 minutes in this experimental result).
- NNN and NAT in the collection solution significantly increased when the treatment time exceeded the timing at which the nicotine concentration in the tobacco raw material reached 0.6% by weight (120 minutes in this experimental result).
- the heating treatment (S20) and the collection treatment (S30) are performed before the timing when the nicotine concentration in the tobacco raw material reaches 0.3% by weight. ) was confirmed to be preferable. That is, it was confirmed that the second condition is preferably a condition that the nicotine concentration in the tobacco raw material decreases until reaching 0.3% by weight.
- the heating process (S20) and the collection process (S30) may be terminated before the timing when the nicotine concentration in the tobacco raw material reaches 0.4% by weight. It was confirmed that it was preferable. That is, it was confirmed that the second condition is more preferably a condition that the nicotine concentration in the tobacco raw material decreases until it reaches 0.4% by weight.
- sample A it is confirmed that it is more preferable to finish the heating process (S20) and the collection process (S30) before the timing when the nicotine concentration in the tobacco raw material reaches 0.6% by weight. It was done. That is, it was confirmed that the second condition is more preferably a condition that the nicotine concentration in the tobacco raw material is decreased until it reaches 0.6% by weight.
- the second condition is more preferably a condition in which the nicotine concentration in the tobacco raw material decreases until it reaches 0.7% by weight. It should be noted that if such a second condition is set, even in the sample A, NNN and NAT in the collection solution do not increase.
- sample P to Q were prepared, and the pH of the collection solution and the concentration of alkaloid (here, nicotine component) contained in the collection solution were measured under the following conditions.
- Sample P is a sample using glycerin as a collection solvent.
- Sample Q is a sample using water as a collection solvent.
- Sample R is a sample using ethanol as a collection solvent.
- the measurement result of the pH of the collection solution is as shown in FIG.
- the measurement result of the concentration of the nicotine component contained in the collection solution is as shown in FIG.
- process time is the time which passed since starting the heat processing (S20) of a tobacco raw material. You may think that processing time is the time which passed since the collection processing (S30) of a nicotine component was started.
- the gas used in the bubbling process is an atmosphere of about 20 ° C. and about 60% -RH.
- the temperature of the collection solvent is a set temperature of a chiller (a constant temperature bath) that controls the temperature of the container that stores the collection solvent. It should be noted that under the present experimental conditions, the temperature of the collection solvent converges about 60 minutes after the container is set in the chiller and the temperature control is started.
- the method was performed in accordance with the German Standardization Organization DIN 10373. That is, 250 mg of tobacco raw material was collected, 7.5 mL of an 11% aqueous sodium hydroxide solution and 10 mL of hexane were added, and the mixture was extracted by shaking for 60 minutes. After extraction, the supernatant hexane phase was subjected to a gas chromatograph mass spectrometer (GC / MS), and the weight of nicotine contained in the tobacco material was quantified.
- GC / MS gas chromatograph mass spectrometer
- the weight of the tobacco raw material in the dry state is calculated by subtracting the above-described moisture content from the total weight of the tobacco raw material.
- GC analysis conditions The conditions of GC analysis used in the measurement of the nicotine component and the amount of water contained in the tobacco raw material are as shown in the following table.
- a method for extracting a flavor component for example, alkaloid containing a nicotine component
- a method for producing a component of a favorite product by extracting a flavor component with a simple device it is possible to provide a method for extracting a flavor component (for example, alkaloid containing a nicotine component) and a method for producing a component of a favorite product by extracting a flavor component with a simple device.
- a flavor component for example, alkaloid containing a nicotine component
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Abstract
Description
実施形態に係る香喫味成分の抽出方法は、たばこ原料から香喫味成分を抽出する抽出方法である。抽出方法は、アルカリ処理が施されたたばこ原料を加熱する工程Aと、第1条件が満たされてから第2条件が満たされるまでのいずれかのタイミングまで、前記工程Aで気相中に放出される放出成分を常温の捕集溶媒に接触させる工程Bとを備える。前記たばこ原料に含まれる糖類の含有量の合計は、乾燥状態において、前記たばこ原料の総重量が100重量%である場合に、9.0重量%以下である。前記第1条件は、前記工程Aを開始してから経過する時間軸上において、前記捕集溶媒及び前記放出成分を含む捕集溶液のpHが極大値から0.2以上減少した後において、前記捕集溶液のpHの変動量が所定範囲内に収まる安定区間が存在する場合に、前記工程Aを開始してから経過する時間が前記安定区間の開始タイミングに達する条件である。前記第2条件は、乾燥状態において、前記たばこ原料の重量が100重量%である場合に、前記たばこ原料に含まれる前記香喫味成分の指標であるニコチン成分の残存量が0.3重量%に達するまで減少する条件である。
(抽出装置)
以下において、第1実施形態に係る抽出装置について説明する。図1及び図2は、第1実施形態に係る抽出装置の一例を示す図である。
以下において、たばこ原料50から抽出された香喫味成分の適用例について説明する。図3は、香喫味成分の適用例を説明するための図である。例えば、香喫味成分は、嗜好品の構成要素(例えば、香味吸引具の香味源)に付与される。
以下において、第1実施形態に係る抽出方法について説明する。図4は、第1実施形態に係る抽出方法を示すフロー図である。
第1実施形態では、放出成分を捕集溶媒70に接触させるステップS30は、少なくとも、第1条件が満たされまで継続する。これによって、放出成分に含まれるアンモニウムイオン(NH4 +)が捕集溶液から十分に除去される。また、たばこ原料50からの放出及び捕集溶媒での抽出において、アンモニウムイオンと同様の挙動を示す他の揮発性夾雑成分(具体的には、アセトアルデヒド、ピリジン)も、第1条件を満たすことによって捕集溶液から除去される。
本発明は上述した実施形態によって説明したが、この開示の一部をなす論述及び図面は、この発明を限定するものであると理解すべきではない。この開示から当業者には様々な代替実施形態、実施例及び運用技術が明らかとなろう。
(第1実験)
第1実験では、図5に示すサンプル(サンプルA~サンプルD)を準備して、以下の条件下において、捕集溶液のpH及び捕集溶液に含まれるアンモニウムイオン(NH4 +)を測定した。
・たばこ原料の量:500g
・たばこ原料の加熱温度:120℃
・アルカリ処理後のたばこ原料のpH:9.6
・アルカリ処理後のたばこ原料の初期水分量:39%±2%
・捕集溶媒の種類:グリセリン
・捕集溶媒の温度:20℃
・捕集溶媒の量:61g
・バブリング処理(通気処理及び捕集処理)時の通気流量:15L/min
第2実験では、バーレー種のたばこ原料のサンプル(上述したサンプルA及びサンプルD)を準備して、以下の条件下において、乾燥状態におけるたばこ原料に含まれるアルカロイド(ここでは、ニコチン成分)の残存量(以下、たばこ原料中ニコチン濃度)、捕集溶液に含まれるアルカロイド(ここでは、ニコチン成分)の回収率(以下、ニコチン回収率)、捕集溶液に含まれるTSNAの濃度(以下、捕集溶液TSNA濃度)を測定した。
・たばこ原料の量:500g
・たばこ原料の加熱温度:120℃
・アルカリ処理後のたばこ原料のpH:9.6
・アルカリ処理後のたばこ原料の初期水分量:39%±2%
・捕集溶媒の種類:グリセリン
・捕集溶媒の温度:20℃
・捕集溶媒の量:60g
・バブリング処理(通気処理及び捕集処理)時の通気流量:15L/min
第3実験では、サンプルP~サンプルQを準備して、以下の条件下において、捕集溶液のpH及び捕集溶液に含まれるアルカロイド(ここでは、ニコチン成分)の濃度を測定した。サンプルPは、捕集溶媒としてグリセリンを用いたサンプルである。サンプルQは、捕集溶媒として水を用いたサンプルである。サンプルRは、捕集溶媒としてエタノールを用いたサンプルである。捕集溶液のpHの測定結果は、図12に示す通りである。捕集溶液に含まれるニコチン成分の濃度の測定結果は、図13に示す通りである。図12及び図13において、処理時間は、たばこ原料の加熱処理(S20)を開始してから経過した時間である。処理時間は、ニコチン成分の捕集処理(S30)を開始してから経過した時間であると考えてもよい。
・たばこ原料の量:500g
・たばこ原料の種類;バーレー種
・たばこ原料の加熱温度:120℃
・アルカリ処理後のたばこ原料のpH:9.6
・捕集溶媒の温度:20℃
・捕集溶媒の量:60g
・バブリング処理(通気処理及び捕集処理)時の通気流量:15L/min
第4実験では、以下の条件下において、捕集溶媒の温度を変更することによって、捕集溶液に含まれるアンモニウムイオン及びピリジンの重量を測定した。捕集溶液に含まれるアンモニウムイオンの重量は、図14に示す通りである。捕集溶液に含まれるピリジンの重量は、図15に示す通りである。
・たばこ原料の量:500g
・たばこ原料の種類;バーレー種
・たばこ原料の加熱温度:120℃
・アルカリ処理後のたばこ原料のpH:9.6
・捕集溶媒の種類:グリセリン
・捕集溶媒の量:60g
(捕集溶液のpHの測定方法)
捕集溶液を22℃の室温でコントロールされた実験室内で、室温になるまで密閉容器内で放置して温度調和した。調和後、ふたを開けて、pHメーター(METTLER TOLEDO社製:セブンイージーS20)のガラス電極を捕集溶液に浸して測定を開始した。pHメーターは、あらかじめpH4.01、6.87、9.21のpHメーター校正液にて校正した。センサーからの出力変動が5秒間で0.1mV以内に安定した点を、その捕集溶液のpHとした。
捕集溶液を50μL採取し、0.05Nの希硫酸水溶液950μLを添加することで希釈し、イオンクロマトグラフィーで分析し、捕集溶液に含まれるアンモニウムイオンを定量した。
ドイツ標準化機構DIN 10373に準ずる方法で行った。すなわち、たばこ原料を250mg採取し、11%水酸化ナトリウム水溶液7.5mLとヘキサン10mLを加え、60分間振とう抽出した。抽出後、上澄みであるヘキサン相をガスクロマトグラフ質量分析計(GC/MS)に供し、たばこ原料に含まれるニコチン重量を定量した。
たばこ原料を250mg採取し、エタノール10mLを加え、60分間振とう抽出を行った。抽出後、抽出液を0.45μmのメンブレンフィルタでろ過し、熱伝導度検出器を備えたガスクロマトグラフ(GC/TCD)に供し、たばこ原料に含まれる水分量を定量した。
捕集溶液を0.5mL採取し、0.1Mの酢酸アンモニウム水溶液9.5mLを添加することで希釈し、高速液体クロマトグラフ質量分析計(LC-MS/MS)にて分析し、捕集溶液に含まれるTSNAを定量した。
たばこ原料に含まれるニコチン成分及び水分量の測定で用いるGC分析の条件は、以下の表に示す通りである。
捕集溶液を1mL採取し、メタノール19mLを添加することで希釈し、希釈した溶液をガスクロマトグラフ質量分析計に供し、捕集溶液に含まれるピリジン量を定量した。
Claims (7)
- たばこ原料から香喫味成分を抽出する香喫味成分の抽出方法であって、
アルカリ処理が施されたたばこ原料を加熱する工程Aと、
第1条件が満たされてから第2条件が満たされるまでのいずれかのタイミングまで、前記工程Aで気相中に放出される放出成分を常温の捕集溶媒に接触させる工程Bとを備え、
前記たばこ原料に含まれる糖類の含有量の合計は、乾燥状態において、前記たばこ原料の総重量が100重量%である場合に、9.0重量%以下であり、
前記第1条件は、前記工程Aを開始してから経過する時間軸上において、前記捕集溶媒及び前記放出成分を含む捕集溶液のpHが極大値から0.2以上減少した後において、前記捕集溶液のpHの変動量が所定範囲内に収まる安定区間が存在する場合に、前記工程Aを開始してから経過する時間が前記安定区間の開始タイミングに達する条件であり、
前記第2条件は、乾燥状態において、前記たばこ原料の重量が100重量%である場合に、前記たばこ原料に含まれる前記香喫味成分の指標であるニコチン成分の残存量が0.3重量%に達するまで減少する条件であることであることを特徴とする抽出方法。 - 前記第2条件は、乾燥状態において、前記たばこ原料の重量が100重量%である場合に、前記たばこ原料に含まれる前記ニコチン成分の残存量が0.4重量%に達するまで減少する条件であることを特徴とする請求項1に記載の抽出方法。
- 前記第2条件は、乾燥状態において、前記たばこ原料の重量が100重量%である場合に、前記たばこ原料に含まれる前記ニコチン成分の残存量が0.6重量%に達するまで減少する条件であることを特徴とする請求項1に記載の抽出方法。
- 前記第2条件は、乾燥状態において、前記たばこ原料の重量が100重量%である場合に、前記たばこ原料に含まれる前記ニコチン成分の残存量が0.7重量%に達するまで減少する条件であることを特徴とする請求項1に記載の抽出方法。
- 前記工程Aにおいて、前記たばこ原料に対して加水処理を施すことを特徴とする請求項1乃至請求項4のいずれかに記載の抽出方法。
- 前記たばこ原料は、バーレー種のたばこ原料であることを特徴とする請求項1乃至請求項5のいずれかに記載の抽出方法。
- 嗜好品の構成要素の製造方法であって、
アルカリ処理が施されたたばこ原料を加熱する工程Aと、
第1条件が満たされてから第2条件が満たされるまでのいずれかのタイミングまで、前記工程Aで気相中に放出される放出成分を常温の捕集溶媒に接触させて、捕集溶液を得る工程Bと、
前記捕集溶液を前記構成要素に添加する工程Cとを備え、
前記たばこ原料に含まれる糖類の含有量の合計は、乾燥状態において、前記たばこ原料の総重量が100重量%である場合に、9.0重量%以下であり、
前記第1条件は、前記工程Aを開始してから経過する時間軸上において、前記捕集溶媒及び前記放出成分を含む捕集溶液のpHが極大値から0.2以上減少した後において、前記捕集溶液のpHの変動量が所定範囲内に収まる安定区間が存在する場合に、前記工程Aを開始してから経過する時間が前記安定区間の開始タイミングに達する条件であり、
前記第2条件は、乾燥状態において、前記たばこ原料の重量が100重量%である場合に、前記たばこ原料に含まれる前記ニコチン成分の残存量が0.3重量%に達するまで減少する条件であることであることを特徴とする製造方法。
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WO2022024307A1 (ja) | 2020-07-30 | 2022-02-03 | 日本たばこ産業株式会社 | 香味成分の抽出方法及び加工済たばこ葉の構成要素の製造方法 |
JP2022534865A (ja) * | 2019-06-05 | 2022-08-04 | フィリップ・モーリス・プロダクツ・ソシエテ・アノニム | 湿潤たばこ抽出物の濃縮 |
JP2022534870A (ja) * | 2019-06-05 | 2022-08-04 | フィリップ・モーリス・プロダクツ・ソシエテ・アノニム | 液体たばこ抽出物、これを作製するための方法およびこれを備えたエアロゾル発生物品 |
JP2022534871A (ja) * | 2019-06-05 | 2022-08-04 | フィリップ・モーリス・プロダクツ・ソシエテ・アノニム | ニコチン組成物、その製造方法、およびそれを備えたエアロゾル発生物品 |
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JP2022534865A (ja) * | 2019-06-05 | 2022-08-04 | フィリップ・モーリス・プロダクツ・ソシエテ・アノニム | 湿潤たばこ抽出物の濃縮 |
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JP2022534871A (ja) * | 2019-06-05 | 2022-08-04 | フィリップ・モーリス・プロダクツ・ソシエテ・アノニム | ニコチン組成物、その製造方法、およびそれを備えたエアロゾル発生物品 |
JP7436517B2 (ja) | 2019-06-05 | 2024-02-21 | フィリップ・モーリス・プロダクツ・ソシエテ・アノニム | 液体たばこ抽出物、これを作製するための方法およびこれを備えたエアロゾル発生物品 |
JP7436518B2 (ja) | 2019-06-05 | 2024-02-21 | フィリップ・モーリス・プロダクツ・ソシエテ・アノニム | ニコチン組成物、その製造方法、およびそれを備えたエアロゾル発生物品 |
WO2022024307A1 (ja) | 2020-07-30 | 2022-02-03 | 日本たばこ産業株式会社 | 香味成分の抽出方法及び加工済たばこ葉の構成要素の製造方法 |
JPWO2022024307A1 (ja) * | 2020-07-30 | 2022-02-03 | ||
JP7342277B2 (ja) | 2020-07-30 | 2023-09-11 | 日本たばこ産業株式会社 | 香味成分の抽出方法及び加工済たばこ葉の構成要素の製造方法 |
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EP3111784B1 (en) | 2018-09-26 |
PL3111784T3 (pl) | 2019-04-30 |
ES2693227T3 (es) | 2018-12-10 |
KR101821080B1 (ko) | 2018-03-08 |
TW201538089A (zh) | 2015-10-16 |
CA2940680C (en) | 2019-01-22 |
RU2639111C1 (ru) | 2017-12-19 |
CN106028844A (zh) | 2016-10-12 |
CN106028844B (zh) | 2018-03-09 |
CA2940680A1 (en) | 2015-09-03 |
US11064726B2 (en) | 2021-07-20 |
JPWO2015129679A1 (ja) | 2017-03-30 |
KR20160110997A (ko) | 2016-09-23 |
US20160360780A1 (en) | 2016-12-15 |
EP3111784A1 (en) | 2017-01-04 |
EP3111784A4 (en) | 2017-09-27 |
JP6101859B2 (ja) | 2017-03-22 |
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