EP2957185B1 - Oral tobacco product - Google Patents
Oral tobacco product Download PDFInfo
- Publication number
- EP2957185B1 EP2957185B1 EP14776038.3A EP14776038A EP2957185B1 EP 2957185 B1 EP2957185 B1 EP 2957185B1 EP 14776038 A EP14776038 A EP 14776038A EP 2957185 B1 EP2957185 B1 EP 2957185B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- tobacco
- raw material
- heating
- tobacco raw
- carried out
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 235000019505 tobacco product Nutrition 0.000 title claims description 46
- 241000208125 Nicotiana Species 0.000 claims description 220
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims description 219
- 239000002994 raw material Substances 0.000 claims description 118
- 238000010438 heat treatment Methods 0.000 claims description 94
- 238000000034 method Methods 0.000 claims description 64
- 239000000284 extract Substances 0.000 claims description 48
- 238000002835 absorbance Methods 0.000 claims description 24
- 102000004190 Enzymes Human genes 0.000 claims description 22
- 108090000790 Enzymes Proteins 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 230000002255 enzymatic effect Effects 0.000 claims description 11
- 239000007858 starting material Substances 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 9
- 238000003306 harvesting Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 description 39
- 230000000694 effects Effects 0.000 description 17
- 238000005259 measurement Methods 0.000 description 15
- 239000000243 solution Substances 0.000 description 11
- 238000004108 freeze drying Methods 0.000 description 9
- 210000000214 mouth Anatomy 0.000 description 7
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- XKLJHFLUAHKGGU-UHFFFAOYSA-N nitrous amide Chemical compound ON=N XKLJHFLUAHKGGU-UHFFFAOYSA-N 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- 241000208134 Nicotiana rustica Species 0.000 description 5
- 239000003086 colorant Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000004806 packaging method and process Methods 0.000 description 5
- 239000008057 potassium phosphate buffer Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 235000019504 cigarettes Nutrition 0.000 description 4
- 238000004737 colorimetric analysis Methods 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 239000004745 nonwoven fabric Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229920002301 cellulose acetate Polymers 0.000 description 2
- 230000001055 chewing effect Effects 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000012460 protein solution Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 241000014040 Melitta Species 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- JVMRPSJZNHXORP-UHFFFAOYSA-N ON=O.ON=O.ON=O.N Chemical compound ON=O.ON=O.ON=O.N JVMRPSJZNHXORP-UHFFFAOYSA-N 0.000 description 1
- 102000004316 Oxidoreductases Human genes 0.000 description 1
- 108090000854 Oxidoreductases Proteins 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000001056 green pigment Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920006389 polyphenyl polymer Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 210000003296 saliva Anatomy 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 238000002525 ultrasonication Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Images
Classifications
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B13/00—Tobacco for pipes, for cigars, e.g. cigar inserts, or for cigarettes; Chewing tobacco; Snuff
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
Definitions
- the present invention relates to an oral tobacco product.
- the tobacco raw material is contained in a packaging medium formed of a material such as nonwoven fabric.
- the user uses the product by placing it in the mouth.
- Patent Documents 1 to 3 describe art for lowering the amount of nitrosamine contained in tobacco raw material when manufacturing oral tobacco products.
- Patent Document 1 describes a method which, in order to reduce the amount of nitrosamine present in tobacco raw material, carries out treatment that includes the step of irradiating tobacco leaves with microwaves, thereby blocking the subsequent formation of nitrosamine in the tobacco leaves.
- Patent Document 2 discloses treatment for lowering the amount of nitrosamine by pressing the harvested tobacco leaves and carrying out steam treatment.
- Patent Document 3 discloses art in which air-dried, yellowed tobacco leaves are dried by a natural drying step and a controlled drying step, lowering the amounts of nitrite nitrogen and nitrosamine in the tobacco raw material.
- Patent Document 4 describes art relating to a smokeless cigarette composition and mentions a coloring agent as being included in the composition.
- Naswar - Wikipedia the free encyclopedia describes Naswar as a green powder comprising sun-dired and air-died tobacco.
- Patent document US 2010/154810 describes the heat treatment of green tobacco for a time sufficient to prevent the formation of at least one nitrosamine.
- the inventor has found that when this tobacco is used as the raw material for oral tobacco products, depending on the treatment conditions, the tobacco remains green even after treatment and extracts thereof which enter the oral cavity are light-colored.
- a coloring agent is mentioned as a material that is included in a smokeless cigarette composition.
- a smokeless cigarette composition may be imparted with color, but the coloring action arises from the coloring agent.
- the object of this invention is to provide an oral tobacco product in which the green color of the tobacco starting material is maintained without using a coloring agent, and which, when extraction is carried out using water as the solvent, gives a light-colored extract.
- the invention provides an oral tobacco product for which the extract that enters the oral cavity of the user at the time of use is not dark-colored.
- the tobacco raw material making up the oral tobacco product retains a green color.
- the type of tobacco serving as the tobacco raw material used in the oral tobacco product of the invention is exemplified by the following genus Nicotiana varieties: the flue-cured and burley varieties of N. tabacum, and the brasilia variety of N. rustica.
- the tobacco leaves used as the tobacco raw material are furnished to the treatment steps shown below before their color turns yellow; that is, when the leaves are for the most part green.
- the phrase "to turn yellow” means that a great majority (e.g., 60% or more, or even 90% or more) of the surface area of the harvested leaf has changed color to a degree where the a* value expressed by the L*a*b* method becomes a value larger than 1.0.
- the (green) pigment present in tobacco leaf decreases after the leaf has been harvested, causing the tobacco leaf to turn yellow.
- the a* value after harvesting of the tobacco leaf is generally from about -9 to about -1.5.
- the tobacco raw material used in the oral tobacco product of the invention has an a* value (or greenness), expressed by the L*a*b* method, of 1.0 or less and an extract of this tobacco raw material, obtained using water as the extracting solvent, has a 420 nm wavelength light absorbance of 1.0 or less.
- the tobacco raw material used in the oral tobacco product of the invention is not particularly limited so long as it satisfies the above conditions.
- the portion of the tobacco leaf from which the midrib has been removed may be furnished to the treatment operations.
- the tobacco leaf may have moisture removed by pressing or the like, then be furnished to the treatment operations.
- the tobacco leaf may be refrigerated or frozen and stored, and subsequently furnished to the treatment operations.
- the green color can be made stronger by harvesting the tobacco leaf at an earlier stage than when the tobacco leaf is to be used in ordinary cigarettes. Having the lower limit of the range in the a* value be -20 or above is suitable from the standpoint of ensuring the green color of the tobacco raw material. In cases where one wishes to make the green color of the tobacco raw material stronger, it is suitable to have the greenness (a* value) be -2 or below.
- Measurement of the a* value of the tobacco raw material can be carried out by using a grinding mill to grind to a size of from 1 to 2 mm (mesh) tobacco raw material that has been dried to a moisture content of 3 to 5 wt %, and the color of the ground sample can be measured using a spectrophotometer.
- the color definitions are those expressed in the L*a*b* color space used by the Commission International de l'Eclairage (CIE) and JIS.
- a numerical result can be obtained by pouring the sample powder into a glass vessel to a layer thickness of 1 cm, directing a standard light (Standard Illuminant D65 for colorimetry, a standard illuminant defined by the CIE and the ISO) at the sample from the bottom of the vessel, and measuring the reflected light (reflected color measurement/specular component excluded (SCE) method).
- a standard light Standard Illuminant D65 for colorimetry, a standard illuminant defined by the CIE and the ISO
- SCE reflected color measurement/specular component excluded
- the a* value can be adjusted by varying the heat treatment temperature and time in the subsequently described tobacco raw material treatment operations.
- a rise in the a* value can be suppressed by lowering the temperature or shortening the time of heat treatment.
- Measurement of the a* value of the tobacco leaf prior to treatment is carried out as follows.
- the color at 20 places on the surface of a tobacco leaf is measured using a spectrophotometer (KONICA MINOLTA/CM3500d, from Konica Minolta Holdings, Inc.). Color definitions, as with the above-described color measurement of the tobacco raw material, is expressed in the L*a*b* color system.
- the 20 places on the surface of the tobacco leaf are uniformly selected at, for example, the center and peripheral portions of the tobacco leaf, as indicated by the stars ( ⁇ ) in FIG. 6 .
- the color measurement operation is carried out by directing a standard light (Standard Illuminant D65 for colorimetry, a standard illuminant defined by the CIE and the ISO) at the sample and measuring the reflected light (reflected color measurement/specular component excluded (SCE) method), and the results are rendered into numerical values.
- a standard light Standard Illuminant D65 for colorimetry, a standard illuminant defined by the CIE and the ISO
- SCE reflected color measurement/specular component excluded
- an extract of the inventive tobacco raw material which is obtained using water as the extracting solvent has a 420 nm wavelength light absorbance (also indicated herein as "ABS 420 nm") of 1.0 or less.
- this absorbance is generally 0.2 or more.
- the extract is obtained by carrying out a procedure such as the following.
- One part by weight of tobacco raw material obtained by lowering the moisture content to 5 wt % or less and grinding is weighed out and added to 25 parts by weight of 22°C water, and shaking extraction is carried out for about 10 minutes.
- the extract is then left to stand at the same temperature for about 20 minutes, after which it is filtered with a 0.20 ⁇ m membrane filter.
- the filtered extract is diluted two-fold with water and the 420 nm wavelength light absorbance is measured using an absorption spectrophotometer.
- the numerical value of the absorbance measured under these conditions is also called the "degree of browning"; a larger numerical value indicates a higher degree of brownness.
- degree of browning a larger numerical value indicates a higher degree of brownness.
- brown-colored are synonymous.
- This degree of browning can be adjusted by varying the heat treatment temperature and time in the subsequently described tobacco raw material treatment operation.
- the oral tobacco product of the invention is exemplified by snus, gum, chewing tobacco, snuff, compressed tobacco (tablets, sticks, etc.), and edible films.
- the oral tobacco product of the invention can be obtained by, for example, the following treatment method.
- the tobacco raw material used in the oral tobacco product of the invention is obtained by a treatment method that includes the step of heating the tobacco raw material under conditions that deactivate an enzyme eliciting enzymatic browning contained therein and the step of lowering the moisture content of the tobacco raw material.
- the prior art described above includes the step of, after the harvested tobacco leaf has turned yellow, drying the yellowed leaf.
- the color of an extract of the tobacco raw material becomes darker.
- the extract has a colorimetric value (ABS 420 nm) of typically about 1.4 or above.
- the treatment step is carried out before the color of the tobacco leaf turns yellow.
- condition that deactivate an enzyme eliciting enzymatic browning refers to conditions such that the enzyme activity (polyphenyl oxidase (PPO) activity) value measured using the procedure described below becomes 0.02 U or less.
- PPO polyphenyl oxidase
- the enzyme activity value can be obtained by adding to an absorption spectrophotometer cell and mixing together a solution of enzyme protein extracted from the sample and a potassium phosphate buffer solution (pH 6.0), then adding to the mixture a 10 mM pyrocatechol solution as the substrate, and measuring at 40°C the increase in the 420 nm wavelength light absorbance with respect to a reference.
- a solution obtained by mixing in deionized water instead of the enzyme protein solution may be used as the reference.
- the amount of enzyme that raises the absorbance of the sample ( ⁇ ABS) by 0.01 over a period of one minute is defined as 1 U.
- condition that deactivate an enzyme eliciting enzymatic browning refers to conditions at which the enzyme activity (PPO activity) on the tobacco leaf becomes 0.02 U or less.
- An example of such conditions is heating at from 80 to 100°C.
- the heating time in this case is typically 40 minutes or less, and may be set according to the heating temperature within a range where the a* value does not undergo a large increase.
- an extract of the tobacco raw material can be made light-colored (having a small ABS 420 nm).
- An embodiment in which such heating is carried out at 85°C or more for 10 minutes or less, and especially at 90°C or more for 5 minutes or less, is more preferred, both from the standpoint of the tobacco raw material not changing color and remaining green, and also from the standpoint of the color of the extract remaining light-colored.
- the above-mentioned temperatures do not refer to the temperature setting of the heating apparatus, but rather to the temperature of the heated tobacco leaf itself.
- the above heating step is exemplified by methods carried out by irradiation with microwaves or infrared light, methods carried out by applying steam, methods carried by immersion in hot water, methods carried out by applying hot air (gas-flow heating), and methods that involve direct contact with a medium such as heated metal. Of these, heating by gas-flow heating is preferred from the standpoint of convenience in production.
- the temperature when raising the tobacco leaf to the desired temperature, it is preferable for the temperature to be elevated as quickly as possible and for the length of time that the temperature remains at the temperature levels (from 30°C to 85°C) during temperature rise to be as short as possible. This is to prevent the enzyme eliciting enzymatic browning within the tobacco leaf from working during temperature rise.
- microwave irradiation is carried out at, typically, a frequency of from about 900 to about 2,500 MHz.
- Methods of heating by applying steam to the tobacco leaf are exemplified by methods in which superheated steam, which is vapor obtained by further heating saturated steam at the same pressure to give it a higher temperature than the saturation temperature, is applied to the tobacco leaf or the tobacco leaf is steamed at the saturated vapor pressure, which is a pressure (gauge pressure) of 0.1 MPa or more.
- Methods of carrying out heating by directing hot air at the tobacco leaf are exemplified by the method of, for example, passing a stream of air having a temperature of 90°C or above and a relative humidity of 90% through the tobacco leaf for 10 minutes or less.
- the operations carried out when producing tobacco raw material to be used in the oral tobacco product of the invention include, for example, the step of lowering the moisture content of the tobacco leaf.
- Including not only the above heating step but also the step of lowering the moisture content helps both to maintain the greenness of the tobacco raw material and also to maintain the light color of the tobacco raw material extract.
- Methods of lowering the moisture content of the tobacco leaf include pneumatic drying and freeze drying in which a low-temperature, normal-temperature or high-temperature stream of air is applied to the tobacco leaf which is either at rest or fluidized, drying by irradiation with microwaves or infrared light, and drying by direct contact with a medium such as heated metal.
- heating may be used for drying by the application of a high-temperature stream of air (hot air), drying by means of microwaves or infrared light, and drying by direct contact with a medium such as heated metal.
- a high-temperature stream of air hot air
- microwaves or infrared light drying by means of microwaves or infrared light
- direct contact with a medium such as heated metal.
- the above step in which heating is carried out and the above step in which the moisture content of the tobacco leaf is lowered are both essential for preparing the tobacco raw material of the invention.
- the moisture content of the tobacco raw material becomes 20 wt % or less, preferably 10 wt % or less, and more preferably 5 wt % or less.
- the harvested tobacco leaf is subjected to heating at 85°C or above for 10 minutes or less, following which the moisture content of the tobacco raw material is lowered using a known freeze-drying method.
- the harvested tobacco leaf is irradiated with microwaves so as to bring the tobacco leaf up to 85°C or above, thereby heating and lowering the moisture content for 10 minutes or less.
- the operation of lowering the moisture content of harvested tobacco leaf entails, for example, carrying out freeze-drying so as to bring the moisture content of the tobacco raw material down to 20 wt % or less, preferably 10 wt % or less, and even more preferably 5 wt % or less; then carrying out heating for 10 minutes or less at an actual tobacco leaf temperature of 85°C or more via, for example, condensation heat transfer by heated steam, convective heat transfer by a stream of air, or conductive heat transfer by contact with a high-temperature object such as metal or plastic.
- Method 3 above When Method 3 above is carried out, to suppress a decrease in the green pigment contained in the tobacco leave, it is preferable to carry out the step of lowering the moisture content at a pressure of less than 0.1 MPa and at 37°C or below.
- the pressure is more preferably 0.05 MPa or less, and even more preferably 0.01 MPa or less. This step is more preferably carried out at a temperature of 0°C or less.
- the tobacco leaf used in treatment is used after being harvested and before the a* value (greenness) becomes larger than 1.0.
- the tobacco raw material used in the oral tobacco product of the invention is obtained by treatment that includes, as described above, the step of heating and the step of lowering the moisture content.
- a* value merely raising the greenness (a* value) of the tobacco raw material after drying
- carrying out freeze-drying alone would suffice.
- tobacco raw material obtained by carrying out freeze-drying alone incurs a pronounced decrease in quality after drying and, together with moisture absorption after drying, undergoes browning.
- extracts of tobacco raw materials that have only been freeze-dried undergo pronounced browning.
- the essential features of the invention namely that the tobacco raw material is green in color and that an extract thereof has a low degree of browning, are not satisfied.
- Deactivating an enzyme eliciting enzymatic browning by passing through the step of carrying out the above-described heating is effective as one condition for keeping the extract from turning brown.
- the oral tobacco product of the invention is made into, for example, snus
- this product is obtained by using a known method to fill the above-described tobacco raw material into a packaging medium formed of a material such as nonwoven fabric.
- the snus is obtained by carrying out filling while adjusting the amount of tobacco raw material, and by carrying out sealing using a means such as heat-sealing.
- the packaging medium may be used without any particular limitation, although preferred use may be made of a cellulose-based nonwoven fabric.
- this gum may be obtained by employing a known method to mix the above-described tobacco raw material used in this invention together with a known gum base.
- the proportion by weight of the total amount of tobacco raw material accounted for by the tobacco raw material which has an a* value expressed by the L*a*b* method of 1.0 or less and an extract of which, obtained using water as the extracting solvent, has a 420 nm wavelength light absorbance of 1.0 or less may be suitably adjusted, but is preferably as large as possible, with a proportion of 40 wt % or more being preferred, a proportion of 60 wt % or more being more preferred, a proportion of 80 wt % or more being even more preferred, a proportion of 98 wt % or more being still more preferred, and a proportion of 100 wt % being most preferred.
- the degree to which the tobacco raw material extract turns brown is small, the seepage of brown color to the packaging medium is likely to be suppressed. Also, the color of the tobacco raw material is kept green.
- the perceived color of the appearance was measured by the following procedure.
- a tobacco raw material that was dried to a moisture content of 3 to 5% was ground to a size of 1 to 2 mm mesh using a grinding mill (MiniBlender, from Melitta Japan, Ltd. (Tokyo, Japan)), and the color of the ground sample was measured using a spectrophotometer (KONICA MINOLTA/CM3500d, from Konika Minolta Holdings, Inc.).
- the color definitions were expressed in the L*a*b* color system used by the Commission International de l'Eclairage (CIE) and JIS.
- the vertical axis (a*) in FIG. 1A shows the spectrophotometer data expressed by the L*a*b* method; a smaller a* value indicates a greener color.
- the microwave-dried leaf had a higher degree of greenness than the conventionally dried tobacco leaf.
- drying methods were used as conventional drying, depending on the variety of tobacco leaf.
- the following conventional drying methods were all carried out under normal pressure.
- the harvested tobacco leaf is dried by a step called "flue-curing.”
- flue-curing a step called "flue-curing.”
- the leaf is cured for 3 days in a humidity-controlled drying room at 30 to 50°C, following which it is dried for 2 days at about 70°C, thereby lowering the moisture in the tobacco raw material to 5 wt % or less.
- the harvested tobacco leaf is dried by a step called "air-curing.” Generally, after being harvested, the leaf is dried to a moisture content of 15 wt % or less over a period of 30 to 35 days in a humidity-controlled environment at from the outside temperature to 35°C.
- the harvested tobacco leaf is dried by a step called "sun-air-curing." Generally, after being harvested, the leaf is sun-dried at the outside temperature for a period of about several days to one week.
- the colorings of extracts obtained from the same three types of raw materials as in Experimental Example 1-1 were measured. The results are shown in FIG. 1B .
- the colors of the extracts, as explained above, are expressed by the 420 nm wavelength light absorbance. A higher absorbance (larger Y-axis value) indicates a browner color.
- the degree of browning for the tobacco raw material extracts was measured by the following method.
- Raw material tobacco leaf dried to a moisture content of 5% or less was weighed out in an amount of 0.4 g, then 10 mL of water was added and shaking extraction was carried out for 10 minutes at 22°C. After shaking, the extract was left to stand at 22°C for 20 minutes, then was filtered with a 0.20 ⁇ m pore diameter membrane filter (Whatman PVDF membrane, from GE Healthcare UK, Ltd. (Buckinghamshire, UK)). The resulting solution was diluted two-fold with water, and the 420 nm wavelength light absorbance was measured using a spectrophotometer.
- extracts of tobacco raw materials obtained by microwave drying had a lower degree of browning than did extracts of tobacco raw material obtained by conventional drying.
- Heat treatment was carried out on the tobacco leaf, and the appearance (perceived color) of the tobacco leaf at that time as well as the appearance of the extract (perceived color) were measured.
- the tobacco leaf used here was a freeze-dried Burley.
- Heat Treatment Heating was carried out at from 40 to 100°C for 10 minutes.
- the tobacco leaf used as the starting material was vacuum-packed, then was heat-treated in a hot-water bath.
- the results are shown in FIGS. 2A and 2B . It is apparent from these results (the colorimetric values when the tobacco leaf (the leaf obtained by freeze-drying Burley tobacco) was heated at the respective temperatures for 10 minutes) that the greenness decreases with heating at 80°C or above ( FIG. 2A ). On the other hand, with heating to 85°C or above, the color of an extract of the heat-treated tobacco raw material becomes lighter (the degree of browning becomes lower) ( FIG. 2B ).
- the types of tobacco leaf used were Burley and freeze-dried tobacco.
- Heat treatment conditions Three levels of 80, 90 and 100°C, a heating time of from 1 to 40 minutes, and the same heating method as in Experimental Example 2.
- FIG. 3A shows the color measurement values for the treated raw material when tobacco leaf (freeze-dried Burley leaf) was heat-treated under three conditions-80°C, 90°C and 100°C-for varying heat treatment times. At each of these temperatures, the degree of greenness decreased with the passage of heating time. At a higher heating temperature, the color faded in a shorter time.
- FIG. 3B shows the degree of browning of extracts of the treated raw material when tobacco leaf (freeze-dried Burley leaf) was heat-treated under three conditions-80°C, 90°C and 100°C-for varying heat treatment times. With the passage of the heating time, the degree of browning of the treated raw material was found to be increasingly suppressed.
- FIG. 4A The appearance of the tobacco raw material ( FIG. 4A ) and the appearance of the tobacco raw material extract ( FIG. 4B ) were examined when heat treatment was carried out at various times-namely, before, during or after drying of the tobacco leaf.
- the tobacco leaf used was Burley tobacco, and the treatment method used in the examples was carried out as follows.
- FIGS. 5A and B The results are shown in FIGS. 5A and B .
- the horizontal axis in these graphs represent the proportion (wt %) of tobacco raw material of the invention.
- Flue-cured (FCV) tobacco leaf that had been stored until most of the leaf surface turned yellow was measured with a colorimeter.
- the greenness (a* value) of the portion that turned yellow, which accounts for the majority of the leaf surface was 2.0 ⁇ 0.7.
- the a* value was 5.3 ⁇ 0.1, and the absorbance (ABS 420 nm) was 1.57.
- the tobacco leaf When change has occurred so that the great majority of the tobacco leaf surface (60% or more of the surface area) has a greenness (a* value) larger than 1.0, the tobacco leaf is referred to as "leaf that has turned yellow"; in other words, the advantageous effects of the invention are not obtained unless at least the great majority of the tobacco leaf (60% or more of the surface area) has an a* value that is 1.0 or less.
- the degrees of greenness (a* value) of the tobacco leaf (frozen tobacco leaf) prior to drying of the Burley, flue-cured and N. rustica tobacco used in the experimental examples of the invention were respectively as follows: Burley, - 2.1 ⁇ 0.3; flue-cured, -2.5 ⁇ 0.6; N. rustica , -4.6 ⁇ 0.5.
- PPO activity measurement was carried out using this enzyme protein solution, a 0.1 M potassium phosphate buffer solution (pH 6.0), and a pyrocatechol solution serving as the substrate.
- the activity measurement procedure was as follows. A 0.1 M potassium phosphate buffer solution (900 ⁇ L) and 100 ⁇ L of an enzyme protein extract prepared by the method described above were mixed together within an absorption spectrophotometer cell. As the control, 900 ⁇ L of a 0.1 M potassium phosphate buffer solution and 100 ⁇ L of deionized water were mixed together, and this was used as a reference.
- the enzyme activities of tobacco leaf that had not been heat-treated were 4.64 U (freeze-dried leaf of a Burley variety (Michinoku)) and 6.42 U (freeze-dried leaf of a Burley variety (Burley 21)), whereas the enzyme activity of tobacco raw material that passed through the heating and moisture-lowering steps were all 0.02 U or less. Based on these results, the heat treatment of tobacco leaf can be regarded as effective for deactivating PPO.
- the tobacco raw material included in the oral tobacco product of the invention retains the green color of the tobacco leaf after harvesting and extracts thereof exhibit a light color, discoloration due to seepage of the oral tobacco product color into the mouth of the user can be prevented.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Tobacco Products (AREA)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2013066348 | 2013-03-27 | ||
PCT/JP2014/054497 WO2014156431A1 (ja) | 2013-03-27 | 2014-02-25 | オーラルたばこ製品 |
Publications (3)
Publication Number | Publication Date |
---|---|
EP2957185A1 EP2957185A1 (en) | 2015-12-23 |
EP2957185A4 EP2957185A4 (en) | 2016-07-06 |
EP2957185B1 true EP2957185B1 (en) | 2018-09-26 |
Family
ID=51623428
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP14776038.3A Active EP2957185B1 (en) | 2013-03-27 | 2014-02-25 | Oral tobacco product |
Country Status (6)
Country | Link |
---|---|
EP (1) | EP2957185B1 (zh) |
JP (1) | JP5992093B2 (zh) |
DK (1) | DK2957185T3 (zh) |
ES (1) | ES2693211T3 (zh) |
TW (1) | TWI540973B (zh) |
WO (1) | WO2014156431A1 (zh) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2016043160A1 (ja) * | 2014-09-18 | 2016-03-24 | 日本たばこ産業株式会社 | たばこ原料の製造方法及びオーラルたばこ製品 |
CN104770859B (zh) * | 2015-02-11 | 2019-12-13 | 贵州中烟工业有限责任公司 | 含荞麦属植物颗粒的口含型无烟气烟草制品及其制备方法 |
WO2021220790A1 (ja) * | 2020-04-28 | 2021-11-04 | 日本たばこ産業株式会社 | 加工済葉たばこの製造方法、及び葉たばこの保管方法 |
Family Cites Families (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1339375A (en) * | 1917-03-14 | 1920-05-04 | Buensod Alfred Charles | Method of curing and treating tobacco |
JPH0740905B2 (ja) * | 1989-06-28 | 1995-05-10 | 日本たばこ産業株式会社 | 色彩検出型葉たばこ種別装置 |
US6135121A (en) | 1996-06-28 | 2000-10-24 | Regent Court Technologies | Tobacco products having reduced nitrosamine content |
BR9810060A (pt) | 1997-06-20 | 2002-07-16 | Regent Court Technologies | Processo de tratamento de tabaco para reduzir o teor de nitrosamina, e produtos produzidos por meio deste |
JP3922985B2 (ja) | 2002-08-22 | 2007-05-30 | 日本たばこ産業株式会社 | 空気乾燥種葉たばこの乾燥方法 |
JP5066092B2 (ja) | 2005-09-22 | 2012-11-07 | アール・ジエイ・レイノルズ・タバコ・カンパニー | 無煙タバコ組成物 |
US8616221B2 (en) * | 2007-02-28 | 2013-12-31 | Philip Morris Usa Inc. | Oral pouch product with flavored wrapper |
JP2012000001A (ja) * | 2008-10-10 | 2012-01-05 | Japan Tobacco Inc | シートたばこの加香装置 |
US20100116281A1 (en) * | 2008-11-07 | 2010-05-13 | Jerry Wayne Marshall | Tobacco products and processes |
US8151804B2 (en) * | 2008-12-23 | 2012-04-10 | Williams Jonnie R | Tobacco curing method |
-
2014
- 2014-02-25 WO PCT/JP2014/054497 patent/WO2014156431A1/ja active Application Filing
- 2014-02-25 JP JP2015508193A patent/JP5992093B2/ja active Active
- 2014-02-25 DK DK14776038.3T patent/DK2957185T3/en active
- 2014-02-25 ES ES14776038.3T patent/ES2693211T3/es active Active
- 2014-02-25 EP EP14776038.3A patent/EP2957185B1/en active Active
- 2014-03-10 TW TW103108081A patent/TWI540973B/zh active
Non-Patent Citations (1)
Title |
---|
None * |
Also Published As
Publication number | Publication date |
---|---|
EP2957185A4 (en) | 2016-07-06 |
EP2957185A1 (en) | 2015-12-23 |
JP5992093B2 (ja) | 2016-09-14 |
TWI540973B (zh) | 2016-07-11 |
TW201446159A (zh) | 2014-12-16 |
JPWO2014156431A1 (ja) | 2017-02-16 |
DK2957185T3 (en) | 2019-01-14 |
WO2014156431A1 (ja) | 2014-10-02 |
ES2693211T3 (es) | 2018-12-10 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP5976690B2 (ja) | 乾燥処理されたタバコ及び乾燥処理方法 | |
US10405570B2 (en) | Method of manufacturing tobacco raw material and oral tobacco product | |
DK3232825T3 (en) | AN ORAL, SMOKE-FREE, MOISTURE SNOSE PRODUCT | |
CN109965341A (zh) | 烟草原料 | |
RU2645577C2 (ru) | Способы уменьшения количества одного или нескольких табак-специфичных нитрозаминов в табачном материале | |
EP2882307B1 (en) | Method for making low nitrosamine contents tobacco | |
EP2957185B1 (en) | Oral tobacco product | |
CN104687233A (zh) | 一种桔子香味再造烟叶的制备方法及桔子香味再造烟叶 | |
US20210000159A1 (en) | Oral tobacco product, method for manufacturing packaging material for oral tobacco product, and method for manufacturing oral tobacco product | |
EP3361877B1 (en) | Tea product and a method of producing it | |
CN102771606A (zh) | 一种蓝莓袋泡绿茶 | |
KR100811463B1 (ko) | 녹차꽃차의 제조 방법 | |
EA017663B1 (ru) | Предшественник напитка, содержащий черный листовой чай, и способ его приготовления | |
KR101289317B1 (ko) | 녹차 흑마늘 제조방법 | |
KR100952877B1 (ko) | 헛개차의 제조방법 | |
JP2020068768A (ja) | 粉末茶及び粉末茶組成物の製造方法 | |
JP2004024207A (ja) | 茶葉保存方法及び茶葉保存システム | |
KR20160081762A (ko) | 감초추출액을 이용한 기능성 커피 생두 및 이를 이용한 커피 음료 | |
ES2741647A1 (es) | Metodo de alcalinizacion de cacao y producto de cacao obtenido mediante dicho metodo | |
JP2014515267A (ja) | 緑茶の製造方法 | |
KR20190143068A (ko) | 그라비올라 차의 제조방법 | |
Pornsoongsong | Antioxidant activity of bamboo leaf tea | |
CN105558108A (zh) | 一种鸦茶制作工艺 | |
KR20030021318A (ko) | 녹차찐빵 및 그 제조방법 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
17P | Request for examination filed |
Effective date: 20150917 |
|
AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR |
|
AX | Request for extension of the european patent |
Extension state: BA ME |
|
A4 | Supplementary search report drawn up and despatched |
Effective date: 20160607 |
|
DAX | Request for extension of the european patent (deleted) | ||
RIC1 | Information provided on ipc code assigned before grant |
Ipc: A24B 15/24 20060101ALI20160601BHEP Ipc: A24B 9/00 20060101ALI20160601BHEP Ipc: A24B 3/04 20060101ALI20160601BHEP Ipc: A24B 3/12 20060101ALI20160601BHEP Ipc: A24B 13/00 20060101AFI20160601BHEP |
|
GRAP | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOSNIGR1 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: GRANT OF PATENT IS INTENDED |
|
INTG | Intention to grant announced |
Effective date: 20180509 |
|
GRAS | Grant fee paid |
Free format text: ORIGINAL CODE: EPIDOSNIGR3 |
|
GRAA | (expected) grant |
Free format text: ORIGINAL CODE: 0009210 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE PATENT HAS BEEN GRANTED |
|
AK | Designated contracting states |
Kind code of ref document: B1 Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR |
|
RAP1 | Party data changed (applicant data changed or rights of an application transferred) |
Owner name: JAPAN TOBACCO INC. |
|
REG | Reference to a national code |
Ref country code: GB Ref legal event code: FG4D |
|
RIN1 | Information on inventor provided before grant (corrected) |
Inventor name: YOKOI, MICHINORI Inventor name: NAGAI, ATSUSHI Inventor name: SATO, SHINSUKE |
|
REG | Reference to a national code |
Ref country code: CH Ref legal event code: EP Ref country code: CH Ref legal event code: NV Representative=s name: NOVAGRAAF INTERNATIONAL SA, CH |
|
REG | Reference to a national code |
Ref country code: AT Ref legal event code: REF Ref document number: 1044955 Country of ref document: AT Kind code of ref document: T Effective date: 20181015 |
|
REG | Reference to a national code |
Ref country code: IE Ref legal event code: FG4D |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R096 Ref document number: 602014033064 Country of ref document: DE |
|
REG | Reference to a national code |
Ref country code: SE Ref legal event code: TRGR |
|
REG | Reference to a national code |
Ref country code: ES Ref legal event code: FG2A Ref document number: 2693211 Country of ref document: ES Kind code of ref document: T3 Effective date: 20181210 |
|
REG | Reference to a national code |
Ref country code: DK Ref legal event code: T3 Effective date: 20190106 |
|
REG | Reference to a national code |
Ref country code: NL Ref legal event code: MP Effective date: 20180926 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: LT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20180926 Ref country code: GR Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20181227 Ref country code: BG Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20181226 Ref country code: RS Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20180926 |
|
REG | Reference to a national code |
Ref country code: NO Ref legal event code: T2 Effective date: 20180926 |
|
REG | Reference to a national code |
Ref country code: LT Ref legal event code: MG4D |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: AL Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20180926 Ref country code: HR Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20180926 Ref country code: LV Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20180926 |
|
REG | Reference to a national code |
Ref country code: AT Ref legal event code: MK05 Ref document number: 1044955 Country of ref document: AT Kind code of ref document: T Effective date: 20180926 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: AT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20180926 Ref country code: EE Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20180926 Ref country code: RO Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20180926 Ref country code: CZ Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20180926 Ref country code: NL Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20180926 Ref country code: IS Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20190126 Ref country code: PL Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20180926 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: PT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20190126 Ref country code: SK Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20180926 Ref country code: SM Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20180926 |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R097 Ref document number: 602014033064 Country of ref document: DE |
|
PLBE | No opposition filed within time limit |
Free format text: ORIGINAL CODE: 0009261 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT |
|
26N | No opposition filed |
Effective date: 20190627 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: SI Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20180926 Ref country code: MC Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20180926 Ref country code: LU Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20190225 |
|
REG | Reference to a national code |
Ref country code: BE Ref legal event code: MM Effective date: 20190228 |
|
REG | Reference to a national code |
Ref country code: IE Ref legal event code: MM4A |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: IE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20190225 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: BE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20190228 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: TR Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20180926 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: MT Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20190225 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: CY Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20180926 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: HU Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT; INVALID AB INITIO Effective date: 20140225 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: MK Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20180926 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: FR Payment date: 20221222 Year of fee payment: 10 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: FI Payment date: 20230224 Year of fee payment: 10 Ref country code: DK Payment date: 20230220 Year of fee payment: 10 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: IT Payment date: 20230223 Year of fee payment: 10 |
|
P01 | Opt-out of the competence of the unified patent court (upc) registered |
Effective date: 20230530 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: ES Payment date: 20230427 Year of fee payment: 10 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: DE Payment date: 20240219 Year of fee payment: 11 Ref country code: CH Payment date: 20240301 Year of fee payment: 11 Ref country code: GB Payment date: 20240219 Year of fee payment: 11 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: SE Payment date: 20240219 Year of fee payment: 11 Ref country code: NO Payment date: 20240222 Year of fee payment: 11 |
|
REG | Reference to a national code |
Ref country code: DK Ref legal event code: EBP Effective date: 20240229 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: FI Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20240225 |