EP0991329A1 - Procedes de traitement du tabac visant a reduire la teneur en nitrosamines, et produits resultants - Google Patents

Procedes de traitement du tabac visant a reduire la teneur en nitrosamines, et produits resultants

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Publication number
EP0991329A1
EP0991329A1 EP98929002A EP98929002A EP0991329A1 EP 0991329 A1 EP0991329 A1 EP 0991329A1 EP 98929002 A EP98929002 A EP 98929002A EP 98929002 A EP98929002 A EP 98929002A EP 0991329 A1 EP0991329 A1 EP 0991329A1
Authority
EP
European Patent Office
Prior art keywords
tobacco
radiation
leaves
subjecting
leaf
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.)
Withdrawn
Application number
EP98929002A
Other languages
German (de)
English (en)
Other versions
EP0991329A4 (fr
Inventor
Jonnie R. Williams
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Regent Court Technologies LLC
Original Assignee
Regent Court Technologies LLC
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from US08/879,905 external-priority patent/US6135121A/en
Application filed by Regent Court Technologies LLC filed Critical Regent Court Technologies LLC
Publication of EP0991329A1 publication Critical patent/EP0991329A1/fr
Publication of EP0991329A4 publication Critical patent/EP0991329A4/fr
Withdrawn legal-status Critical Current

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Classifications

    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B3/00Preparing tobacco in the factory
    • A24B3/10Roasting or cooling tobacco
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/22Treatment of tobacco products or tobacco substitutes by application of electric or wave energy or particle radiation

Definitions

  • the present invention relates to a method of treating tobacco to reduce the content of, or prevent formation of, harmful nitrosamines which are normally found m tobacco.
  • the present invention also relates to tobacco products having low nitrosamme content .
  • Patent No. 4,898,189 Wochnowski teaches the use of microwaves to treat green tobacco m order to control moisture content m preparation for storage or shipping.
  • microwave energy is described to kill insect infestation of tobacco.
  • techniques using impregnation of tobacco with inert organic liquids U.S. Patent No. 4,821,747) for the purposes of extracting expanded organic materials by a sluicing means have been disclosed wherein the mixture was exposed to microwave energy.
  • microwave energy is disclosed as the drying mechanism of extruded tobacco- contammg material (U.S. Patent No. 4,874,000).
  • Stungis discloses the use of microwave to dry and expand cigarettes made with wet tobacco.
  • cured tobacco is known to contain a number of nitrosamines, including the harmful carcinogens N' -nitrosonornicotme (NNN) and 4-(N- nitrosomethylammo) -1- (3-py ⁇ dyl) -1-butanone (NNK) . It is widely accepted that such nitrosamines are formed post -harvest , during the curing process, as described further herein. Unfortunately, fresh-cut green tobacco is unsuitable for smoking or other consumption.
  • Wiernik et al includes some of Burton et al's summary data on lamina and midrib nitrite and TSNA contents m the KY160 and KY171 samples. Data from the freeze- drying and the quick-drying tests are included, but there is no mention of the microwaved samples. The article contains the following conclusion:
  • the Weirnik et al article also discusses traditional curing of Skroniowski tobacco m Tru as an example of a 2 -step curing procedure.
  • the article states that the tobacco is first air-cured and, when the lamina is yellow or brownish, the tobacco is heated to 65°C for two days m order to cure the stem.
  • An analysis of tobacco produced m this manner showed that both the nitrite and the TSNA values were low, i.e., less than 10 micrograms per gram and 0.6-2.1 micrograms per grams, respectively.
  • Weirnik et al theorized that these results were explainable due to the rapid heating whicn does not allow further bacterial growth.
  • One object of the present invention is to substantially eliminate or reduce the content of nitrosamines m tobacco intended for smoking or consumption by other means. Another object of the present invention is to reduce the carcinogenic potential of tobacco products, including cigarettes, cigars, chewing tobacco, snuff and tobacco-containing gum and lozenges .
  • Still another object of the present invention is to substantially eliminate or significantly reduce the amount of tobacco-specific nitrosamines, including N' -nitrosonornicotme (NNN) , 4- (N-nitrosomethylammo) -1- (3-pyr ⁇ dyl) -1-butanone (NNK), N' -nitrosoanatabme (NAT) and N' -nitrosoanabasme (NAB) , in such tobacco products.
  • NNN N' -nitrosonornicotme
  • NNK 4- (N-nitrosomethylammo) -1- (3-pyr ⁇ dyl) -1-butanone
  • NAT N' -nitrosoanatabme
  • NAB N' -nitrosoanabasme
  • Another object of the present invention is to treat uncured tobacco at an appropriate time post -harvest so as to arrest the curing process without adversely affecting the tobacco's suitability for human consumption.
  • Another object of the present invention is to reduce the content of tobacco-specific nitrosamines m fully cured tobacco.
  • Yet another object of the present invention is to reduce the content of tobacco-specific nitrosamines, particularly NNN and NNK, and metabolites thereof m humans who smoke, consume or otherwise ingest tobacco m some form, by providing a tobacco product suitable for human consumption which contains a substantially reduced quantity of tobacco-specific nitrosamines, thereby lowering the carcinogenic potential of such product.
  • the tobacco product is a cigarette, cigar, chewing tobacco or a tobacco-contammg gum or lozenge.
  • a process for reducing the amount of or preventing formation of nitrosamines in a harvested tobacco plant comprising subjecting at least a portion of the plant to microwave radiation, while said portion is uncured and m a state susceptible to having the amount of nitrosamines reduced or formation of nitrosamines arrested, for a sufficient time to reduce the amount of or substantially prevent formation of at least one nitrosamme.
  • the step of subjecting to microwave radiation is carried out on a tobacco leaf or portion thereof after onset of yellowing m the leaf and prior to substantial accumulation of tobacco-specific nitrosamines m the leaf. It is also preferred that in the process of the invention, the step of subjecting to microwave radiation is carried out prior to substantial loss of the leaf's cellular integrity.
  • the tobacco is flue tobacco and the step of subjecting to microwave radiation is carried out withm about 24 to about: 72 hours post- harvest, even more preferaoly withm about 24 to about 36 hours post -harvest .
  • the harvested tobacco is maintained under above-ambient temperature conditions m a controlled environment prior to the step of subjecting to microwave radiation.
  • Preferred aspects of the process include a step, prior to subjecting a tobacco leaf which preferably includes the stem to microwave radiation, of physically pressing the leaf to squeeze excess moisture therefrom, to ensure more uniform drying by the microwave unit.
  • This step can be conveniently carried out by passing the leaf through a pair of appropriately spaced rotating cylindrical rollers prior to entering the microwave cavity.
  • the microwave radiation has a frequency of about 900 to about 2500 MHz, and is applied to the plant for a period of at least about 1 second, and preferably from about 10 seconds to about 5 minutes at a predetermined power level.
  • the power level used generally determines the length of time to which the tobacco is subjected to the microwave radiation, and can range from about 600 to about 1000 watts when using conventional kitchen-type microwave ovens, up to several hundred or more kilowatts for commercial, multimode applicators.
  • Preferred power levels using applicators designed to handle single leaves range from about 2 to about 75 kilowatts, more preferably from about 5 to about 50 kilowatts, which permit relatively rapid treatment to be carried out .
  • the microwave radiation is applied to the leaf or portion thereof for a time sufficient to effectively dry the leaf, without charring, so that it is suitable for human consumption.
  • the present invention also seeks to subject tobacco leaves to microwave radiation to prevent normal accumulation of at least one tobacco-specific nitrosamme, such as N' -nitrosonornicotme, 4- (N-nitrosomethylammo) -1- (3-py ⁇ dyl) -1-butanone, N' - nitrosoanatabme and N' -nitrosoanabasme .
  • the present invention m its broadest forms also encompasses a tobacco product comprising non-green tobacco suitable for human consumption and having a lower content of at least one tobacco- specific nitrosamme than conventionally cured tobacco.
  • the non-green tobacco product has a TSNA (NNN, NNK, NAB and NAT) content of less than .2 ⁇ g/g, more preferably less than about .15 ⁇ g/g, and even more preferably less than about .1 ⁇ g/g, an NNN content of less than about .15 ⁇ g/g more preferably less than about .10 ⁇ g/g, and even more preferably less than about .05 ⁇ g/g, and an NNK content of less than about: .002 ⁇ g/g, more preferably less than apout .001 ⁇ g/g, and even more preferably less than about .0005 ⁇ g/g.
  • NNK TSNA
  • the present invention is also directed to a tobacco product comprising dried yellow tobacco suitable for human consumption and having a lower content of at least one tobacco-specific nitrosamme than conventionally cured tobacco.
  • the yellow tobacco product has a TSNA (NNN, NNK, NAB and NAT) content, an NNN content, and an NNK content withm the above preferred ranges.
  • the non-green or yellow tobacco product comprises non-green or yellow tobacco suitable for human consumption, and having a TSNA (NNN, NNK, NAB and NAT) content withm about 25% by weight of the content of such TSNA m the freshly harvested green tobacco crop from which the product was made. It is more preferred that the non-green or yellow tobacco product have a TSNA content withm about 10% by weight, more preferably withm about 5% by weight and most preferably essentially approximating (e.g. withm an amount up to several percent by weight) the content of such TSNA m the freshly harvested tobacco crop from which the product was made.
  • the non-green or yellow tobacco product comprises non-green or yellow tobacco suitable for human consumption, and having content of at least one TSNA selected from NNN, NNK, NAB and NAT, which is withm about 25% by weight, preferably withm about 10% by weight, more preferably withm about 5% by weight and most preferably essentially approximating (e.g. withm an amount up to several percent by weight) of the content of the corresponding TSNA or TSNAs in the freshly harvested green tobacco crop from which the product was made.
  • TSNA selected from NNN, NNK, NAB and NAT
  • the non- green or yellow tobacco product comprises non-green or yellow tobacco suitable for human consumption, and having a TSNA (NNN, NNK, NAB and NAT) content which is at least about 75% by weight, preferably at least about 90% by weight, more preferably at least about 95% by weight, and most preferably at least about 99% by weight lower than the content of such TSNA m a tobacco product of the same type made from the same tobacco crop as the product of the invention, but which was cured m the absence of microwave radiation or other techniques designed to reduce TSNA content.
  • TSNA NNN, NNK, NAB and NAT
  • the non-green or yellow tobacco product comprises non-green or yellow tobacco suitable for human consumption, and having a content of at least one TSNA selected from NNN, NNK, NAB and NAT which is at least about 75% by weight, preferably at least about 90% by weight, more preferably at least about 95% by weight, and most preferably at least about 99% by weight lower than the content of the corresponding TSNA or TSNAs in a tobacco product of the same type made from the same tobacco crop as the product of the invention, but which was cured m the absence of microwave radiation or other techniques designed to reduce TSNA content .
  • TSNA selected from NNN, NNK, NAB and NAT
  • a preferred form of the present invention relates to a tobacco product comprising tobacco having a reduced content of at least one tobacco-specific nitrosamme, produced by a process comprising subjecting the tobacco, while the tobacco is uncured and susceptible to having formation of at least one tobacco- specific nitrosamme arrested, to microwave radiation.
  • the present invention is directed to a method for reducing the content of at least one tobacco- specific nitrosamme m cured brown tobacco, comprising rehydratmg the cured brown tobacco, and subjecting the rehydrated tobacco to microwave radiation at a predetermined energy level for a predetermined length of time.
  • the present invention includes withm its scope a tobacco product comprising cured brown tobacco having a reduced content of at least one tobacco-specific nitrosamme, produced by a process comprising rehydratmg the cured brown tobacco, and subjecting the rehydrated tobacco to microwave radiation at a predetermined energy level for a predetermined length of time.
  • the present invention relates to a method of manufacturing a tobacco product, comprising subjecting harvested tobacco leaves to microwave radiation, while said leaves are uncured and m a state susceptible to having the amount of tobacco-specific nitrosamines reduced or formation of tobacco-specific nitrosamines arrested, for a sufficient time to reduce the amount of or substantially prevent formation of at least one tobacco-specific nitrosamme m the leaves, and forming the tobacco product comprising the microwaved leaves, the tobacco product being selected from cigarettes, cigars, chewing tobacco, snuff and tobacco-containing gum and lozenges .
  • the present invention also relates to a method for reducing the amount of or preventing formation of nitrosamines m a harvested tobacco plant, comprising subjecting at least a portion of the plant to radiation having a frequency higher than the microwave domain, while said portion is uncured and in a state susceptible to having the amount of nitrosamines reduced or formation of nitrosamines arrested, for a sufficient time to reduce the amount of or substantially prevent formation of at least one nitrosamme.
  • the step of subjecting to radiation having a frequency higher than the microwave domain is carried out on a topacco leaf or portion thereof after onset of yellowing m the leaf and prior to substantial accumulation of tobacco- specific nitrosamines the leaf. It is also preferred that m the process of the invention, the step of subjecting to such radiation is carried out prior to substantial loss of the leaf's cellular integrity.
  • Preferred energy sources capable of producing such radiation include far-infrared and infrared radiation, UV (ultraviolet radiation) , soft x-rays or lasers, accelerated particle beams such as electron beams, x-rays and gamma radiation.
  • FIG. 1 is a photograph illustrating "yellow” Virginia flue tobacco aged 24 to 72 hours post -harvest .
  • FIG. 2 is a photograph illustrating low-nitrosamme microwaved "yellow” Virginia flue tobacco m accordance with the present invention.
  • FIG. 3 is a partial, side-perspective illustration of a mobile, commercial-scale microwave applicator which can be employed to carry out the microwave treatment m accordance with the present invention.
  • the present invention is founded on the discovery that a window exists during the tobacco curing cycle, m which the tobacco can be treated in a manner that will essentially prevent the formation of TSNA.
  • m which the tobacco can be treated in a manner that will essentially prevent the formation of TSNA.
  • the precise window aur g which TSNA formation can be effectively eliminated or substantially reduced depends on the type of tobacco, method of curing, and a number of other variables, including those mentioned above.
  • the window corresponds to the time frame post -harvest when the leaf is beyond the fresh-cut or "green” stage, and prior to the time at which TSNAs and/or nitrites substantially accumulate m the leaf; this time frame typically corresponds to the period m which the leaf is undergoing the yellowing process or is m the yellow phase, before the leaf begins to turn brown, and prior to the substantial loss of cellular integrity.
  • the terms "substantial” and “significant” as used herein generally refer to predominant or majority on a relative scale, give or take.
  • the leaves are susceptible to having the formation of TSNAs substantially prevented, or the content of any already formed TSNAs reduced, by exposing the tobacco to microwave radiation at a predetermined energy level for a predetermined length of time, as discussed further below.
  • This microwave treatment essentially arrests the natural formation of TSNAs, and provides a dried, golden yellow leaf suitable for human consumption. If TSNAs have already begun to substantially accumulate, typically toward the end of the yellow phase, the application of microwave energy to the leaf in accordance with the invention effectively arrests the natural TSNA formation cycle, thus preventing any further substantial formation of TSNA.
  • yellow or yellowing tobacco is treated m this fashion at the most optimal time m the curing cycle, the resulting tobacco product has TSNA levels essentially approximating those of freshly harvested green tobacco, while maintaining its flavor and taste.
  • the present invention relates to treatment of cured (brown) tobacco to effectively reduce the TSNA content of that cured tobacco, by rehydratmg cured tobacco and subjecting the rehydrated cured tobacco to microwave radiation, as described further below.
  • the present invention is applicable to treatment of the harvested tobacco which is intended for human consumption.
  • Much research has been performed on tobacco, with particular reference to tobacco-specific nitrosamines.
  • Freshly harvested tobacco leaves are called "green tobacco" and contain no known carcinogens, but green tobacco is not suitable for human consumption.
  • the process of curing green tobacco depends on the type of tobacco harvested. For example, Virginia flue (bright) tobacco is typically flue-cured, whereas Burley and certain dark strains are usually air-cured.
  • flue-curing of tobacco typically takes place over a period of five to seven days compared to one to two+ months for air-curing.
  • flue-curing has generally been divided into three stages: yellowing (35-40°C) for about 36-72 hours (although others report that yellowing begins sooner than 36 hours, e.g., at about 24 hours for certain Virginia flue strains) , leaf drying (40-57°C) for 48 hours, and midrib (stem) drying (57-75°C) for 48 hours.
  • yellowing 35-40°C
  • leaf drying 40-57°C
  • midrib (stem) drying 57-75°C
  • the yellowing stage is carried out m a barn. During this phase the green leaves gradually lose color due to chlorophyll degradation, with the corresponding appearance of the yellow carotenoid pigments.
  • the yellowing stage of flue-curing tobacco is accomplished by closing external air vents in the barn, and holding the temperature at approximately 35°- 37°C. This process utilizes a controlled environment, maintains the relative humidity m the barn at approximately 85%, limits moisture loss from the leaves, and allows the leaf to continue the metabolic processes begun m the field. The operator constantly monitors the progress of the cure, primarily by observing the loss of chlorophyll and green color from the leaves, and the development of the desired lemon to golden orange leaf color.
  • tobacco-specific nitrosamines are formed upon reaction of amines with nitrite-derived nitrosatmg species, such as N0 2 , N 2 0 3 and N 2 0 4 under acidic conditions.
  • nitrite-derived nitrosatmg species such as N0 2 , N 2 0 3 and N 2 0 4 under acidic conditions.
  • Tobacco leaves contain an abundance of amines m the form of amino acids, proteins, and alkaloids.
  • the tertiary a ine nicotine (referenced as (1) m the diagram below) is the major alkaloid m tobacco, while other nicotme-type alkaloids are the secondary amines nornicotine (2), anatabme (3) and anabasme (4) .
  • Tobacco also generally contains up to 5% of nitrate and traces of nitrite.
  • NN N' -nitrosoanatabme
  • NAT N' -nitrosonabas e
  • NNA N-nitrosomethylammo
  • NNK 4- (N-nitrosomethylammo) -1- (3 -py ⁇ dyl) -1- butanone
  • NNA 4- (N-nitrosomethylammo) -4- (3- pyridyl) -1-butanal
  • TSNA 4- (N-nitrosomethylammo) - 1- (3 -pyridyl ) - 1 -butanol ,
  • nitrite and TSNA accumulate on air- cu ⁇ ng at the time intervals starting after the end of yellowing and ending when the leaf turns completely brown, e.g., 2-3 weeks after harvest for certain air-cured strains, and approximately a week or so after harvest m flue-cured varieties. This is the time during which loss of cellular integrity occurs, due to moisture loss and leakage of the content of cells into the intercellular spaces. Therefore, there is a short window time during air- curing when the cells have disintegrated, making the nutrition available for microorganisms. Weirnik et al have suggested that nitrite may then substantially accumulate as a result of dissi ilatory nitrate reduction, thus rendering formation of TSNA possible.
  • the formation of TSNAs tobacco is substantially prevented or arrested by subjecting the harvested leaves to microwave radiation under the conditions described herein.
  • the tobacco leaves are exposed to the microwave energy at a time between the onset of yellowing and the substantial loss of cellular integrity.
  • non-green and/or yellow tobacco products can be obtained which are suitable for human consumption, and which have a lower content of at least one tobacco-specific nitrosamme than conventionally cured tobacco.
  • Green or fresh-cut tobacco is generally unsuitable for human consumption as noted above; "non- green” as used herein means means the tobacco has at least lost the majority of chlorophyll, and includes without limitation partially yellow leaves, full yellow leaves, and leaves which have begun to turn brown in places.
  • the non-green tobacco product has a TSNA (NNN, NNK, NAB and NAT) content of less than .2 ⁇ g/g, more preferably less than about .15 M9/g * an -d even more preferably less than about .1 ⁇ g/g, an NNN content of less than about .15 ⁇ g/g, more preferably less than about .10 ⁇ g/g, and even more preferably less than about .05 ⁇ g/g, and an NNK content of less than about .002 ⁇ g/g, more preferably less than about .001 ⁇ g/g, and even more preferably less than about .0005 ⁇ g/g.
  • TSNA NN, NNK, NAB and NAT
  • the present invention is also directed to a tobacco product comprising dried yellow tobacco suitable for human consumption and having a lower content of at least one tobacco-specific nitrosamme than conventionally cured tobacco.
  • the yellow tobacco product has a TSNA (NNN, NNK, NAB and NAT) content, an NNN content, and an NNK content withm the above preferred ranges .
  • the non-green or yellow tobacco product comprises non-green or yellow tobacco suitable for human consumption, and having a TSNA (NNN, NNK, NAB and NAT) content withm about 25% by weight of the content of such TSNA m the freshly harvested green tobacco crop from which the product was made. It is more preferred that the non-green or yellow tobacco product have a TSNA content withm about 10% by weight, more preferably withm about 5% by weight and most preferably essentially approximating (e.g. withm an amount up to several percent by weight) the content of such TSNA the freshly harvested tobacco crop from which the product was made.
  • TSNA NNN, NNK, NAB and NAT
  • the present invention permits tobacco products to be made which have a TSNA content withm the above-described ranges as to amounts, whereas normally cured tobacco from the same crop would typically generate many times the amount of TSNA m the fresh-cut tobacco.
  • the present invention can effectively lock m the low amounts of nitrosamines found in fresh-cut green tobacco.
  • the non-green or yellow tobacco product comprises non-green or yellow tobacco suitable for human consumption, and having content of at least one TSNA selected from NNN, NNK, NAB and NAT, which is withm about 25% by weight of, preferably with about 10% by weight of, more preferably withm about 5% by weight of, and most preferably essentially approximating (e.g., withm an amount up to several percent by weight) the content of the corresponding TSNA or TSNAs m the freshly harvested green tobacco crop from which the product was made.
  • TSNA selected from NNN, NNK, NAB and NAT
  • the content of, e.g., NNN m the tobacco of the invention falls withm the above ranges vis-a- vis the amount of NNN m the fresh-cut green tobacco, or the amount of NNN + NNK m the tobacco of the invention falls withm the above ranges vis-a-vis the amount of NNN + NNK m the fresh- cut green tobacco, etc.
  • the fresh- cut green tobacco is preferably analyzed for TSNA content withm about 24 hours after harvest.
  • the non- green or yellow tobacco product comprises non-green or yellow tobacco suitable for human consumption, and having a TSNA (NNN, NNK, NAB and NAT) content which is at least about 75% by weight, preferably at least about 90% by weight, more preferably at least about 95% by weight, and most preferably at least about 99% by weight lower than the content of such TSNA m a tobacco product of the same type made from the same tobacco crop as the product of the invention, but which was cured m the absence of microwave radiation or other steps specifically designed to reduce the TSNA content.
  • TSNA NNN, NNK, NAB and NAT
  • the non-green or yellow tobacco product comprises non-green or yellow tobacco suitable for human consumption, and having a content of at least one TSNA selected from NNN, NNK, NAB and NAT which is at least about 75% by weight, preferably at least about 90% by weight, more preferably at least about 95% by weight, and most preferably at least about 99% by weight lower than the content of the corresponding TSNA or TSNAs m a tobacco product of the same type (e.g., comparing a cigarette to another cigarette) made from the same tobacco crop as the product of the invention, but which was cured m the absence of microwave radiation or other techniques for reducing TSNA content.
  • a content of at least one TSNA selected from NNN, NNK, NAB and NAT which is at least about 75% by weight, preferably at least about 90% by weight, more preferably at least about 95% by weight, and most preferably at least about 99% by weight lower than the content of the corresponding TSNA or TSNAs m a tobacco product of
  • the TSNA weight % comparisons can be made by taking, for example, a cigarette made using dried yellow tobacco m accordance with the present invention, and taking a cigarette made from tobacco from the same crop as the dried yellow tobacco was made from, but curing it by conventional means without subjecting it to microwave radiation.
  • the yellow stage in which the step of subjecting the tobacco leaf to microwave radiation is preferaoly carried out, can be broadly defined m any one of the following ways: (a) by examining the color of the leaf, when the green color has substantially given way to a yellowish color; (b) by measuring the percent of chlorophyll conversion to sugars; (c) by observing the onset of either nitrite formation or nitrosamme generation, which typically coincide with the end of the yellow phase, or (d) by measuring the moisture content of the leaves, e.g., when they have a moisture content from about 40 to about 70 percent by weight. If the microwave radiation is applied to green tobacco, the arrestation or prevention of nitrosamme formation is not observed.
  • the optimal time for subjecting the harvested tobacco to the microwave radiation during the yellow phase varies depending on a number of factors, including varietal differences, environmental variations, etc.
  • time frame beginning with onset of yellowing defined, e.g., by a loss of the majority of green color m the leaf
  • time at which the leaf substantially loses cellular integrity as it turns brown
  • one of ordinary skill m the art could determine the optimal time for carrying out the microwave treatment for any given variety of tobacco.
  • sample leaves could be tested by the procedures described herein to measure either nitrite or TSNA content, to identify the relative time m a given cure cycle at which significant TSNA accumulation begins, or identify the transition phase m which loss of cellular integrity occurs.
  • the principles of the invention can also be applied to tobacco leaves which are m the process of forming, and have already accumulated significant amounts of TSNAs. When the microwavmg is carried out at this latter stage, further formation of TSNAs can be effectively arrested.
  • TSNA levels have essentially stabilized, and application of microwave radiation is ineffective to reduce the TSNA context, except under rehydration conditions described below.
  • the tobacco leaf Upon being subjected to microwave radiation m accordance with the present invention, the tobacco leaf generally has a reduced moisture content, i.e. less than about 10% by weight, and often approximately 5%. If desired, the leaf can be rehydrated back to the typical moisture range for brown, cured tobacco (e.g., about 11-15% for Virginia flue) before manufacturing into tobacco products such as cigarettes.
  • a reduced moisture content i.e. less than about 10% by weight, and often approximately 5%.
  • the leaf can be rehydrated back to the typical moisture range for brown, cured tobacco (e.g., about 11-15% for Virginia flue) before manufacturing into tobacco products such as cigarettes.
  • the present invention is applicable to all strains of tobacco, including flue or bright varieties, Burley varieties, dark varieties, oriental/Turkish varieties, etc. Withm the guidelines set forth herein, one of ordinary skill m the art could determine the most efficient time m the cure cycle for carrying out the microwave step to achieve the objects and advantages of the present invention.
  • Preferred aspects of the process include a step, prior to subjecting a tobacco leaf which preferably includes the stem to microwave radiation, of physically pressing the leaf to squeeze excess moisture therefrom, to ensure more uniform drying by the microwave unit.
  • This step can be conveniently carried out by passing the leaf through a pair of appropriately spaced rotating cylindrical rollers prior to entering the microwave cavity.
  • Such a pressing step will aid in wringing moisture from the stem and, to a lesser extent, the midrib and larger veins, and lead to a better and more evenly dried product.
  • the rollers can be made of hard rubber, plastic or steel and be of any desired length, and are preferably spaced about one-eighth to about one-quarter inch apart, but the distance is preferably selected so as to accomodate the thickness of a single leaf, which can vary.
  • the rollers can be belt or chain driven by an appropriately selected motor. Besides rotating rollers, other types of squeezing or pressing means could be used to accomplish the same result, if desired, as would be apparent to one of ordinary skill in
  • the above-described preferred embodiment of pressing the leaves permits more high-speed production to be carried out, since the stems do not have to be cut out, and the microwave time can be reduced.
  • This embodiment is particularly advantageous for tobacco leaves destined to be used m cigarettes, which typically contain some tobacco stems as part of a blend.
  • the pressing step can be omitted if desired, m applications where the stem is trimmed from the leaves and discarded.
  • the leaves instead of pressing the leaves or cutting out the stems, the leaves can be subjected to a steam treatment prior to microwavmg.
  • a steam treatment prior to microwavmg.
  • steaming the whole leaves, including the stems has been demonstrated to more evenly distribute the moisture m the stems and larger veins, thus leading to more uniform drying of the entire leaves upon microwavmg.
  • the entire leaves including the stems can be used m tobacco products when this particular technique is employed
  • successful results have been obtained when the leaves have been placed m a suitable steam vessel for a time sufficient to allow the leaves to become somewhat soft and pliable, generally from about 30 seconds up to about five minutes.
  • the principles of the present invention can also be applied to brown or already cured tobacco, which has been rehydrated.
  • the results are not as dramatic as when the invention is applied to uncured yellow tobacco, prior to the time when substantial quantities of TSNAs or nitrites have accumulated m the leaves.
  • the addition of moisture to the cured leaves such as by spraying with enough water to effectively soak the leaves, followed by microwavmg the rehydrated leaves, reduces the content of TSNAs as demonstrated m the following Examples.
  • the cured tobacco product is rehydrated by adding an appropriate amount of water, generally at least about 10% by weight, up to the maximum absorption capacity, directly to the leaves . Exposure of the rehydrated leaves to microwave radiation, in the same manner as described herein with regard to the uncured tobacco, reduces the nitrosamme content, as shown below.
  • the leaves can be wetted n any suitable fashion.
  • the cured tobacco is m a form other than leaves, such as reconstituted "sheet” tobacco, it can similarly be rehydrated with, e.g., 10-70% by weight water, and then microwaved. Suitable microwave condition can be selected depending on the degree to which the leaves are re-wetted, but typically fall withm the parameters discussed above for microwavmg yellow tobacco.
  • microwavmg of the rehydrated brown tobacco can preferably reduce the TSNA (NNN, NNK, NAB and NAT) content, measured individually or collectively, by at least about 25% by weight, more preferaply by at least about 35% by weight, and even more preferably by at least about 50% by weight from the TSNA levels contained the cured brown tobacco prior to rehydration.
  • TSNA TSNA
  • microwave radiation refers to electromagnetic energy m the form of microwaves having a frequency and wavelength typically characterized as falling withm the microwave domain.
  • microwave generally refers to that portion of the electromagnetic spectrum which lies between the far- infrared region and the conventional radiofrequency spectrum.
  • the range of microwaves extends from a wavelength of approximately 1 millimeter and frequency of about 300,000 MHz to wavelength of 30 centimeters and frequency of slightly less than about 1,000 MHz.
  • the present invention preferably utilizes high power applications of microwaves, typically at the lower end of this frequency range.
  • microwaves due to a greater penetration, microwaves generally heat quickly to a depth several centimeters while heating by infrared is much more superficial.
  • infrared for example, m cooking
  • commercial microwave apparatuses such as kitchen microwave ovens, are available at standard frequencies of approximately 915 MHz and 2450 MHz, respectively. These frequencies are standard industrial bands.
  • microwave frequencies of 2450 and 896 MHz are commonly employed. Under properly balanced conditions, however, microwaves of other frequencies and wavelengths would be useful to achieve the objects and advantages of the present invention.
  • Microwave energy can be generated at a variety of power levels, depending on the desired application.
  • Microwaves are typically produced by magnatrons, at power levels of 600-1000 watts for conventional kitchen-level microwave apparatuses (commonly at about 800 watts) , but commercial units are capable of generating power up to several hundred kilowatts, generally by addition of modular sources of about 1 kilowatt .
  • a magnatron can generate either pulsed or continuous waves of suitably high frequency.
  • the applicator is a necessary link between the microwave power generator and the material to be heated.
  • any desired applicator can be used, so long as it is adapted to permit the tobacco plant parts to be effectively subjected to the radiation.
  • the applicator should be matched to the microwave generator to optimize power transmission, and should avoid leakage of energy towards the outside.
  • Multimode cavities microwave ovens
  • the applicator can be equipped with a mode stirrer (a metallic moving device which modifies the field distribution continuously), and with a moving table surface, such as a conveyor belt. The best results are attained by single leaf thickness exposure to microwave radiation, as opposed to stacks or piles of leaves.
  • the microwave conditions comprise microwave frequencies of about 900 MHz to about 2500 MHz, more preferably about 915 MHz and about 2450 MHz, power levels of from about 600 watts up to 300 kilowatts, more preferably from about 600 to about 1000 watts for kitchen-type applicators and from about 2 to about 75 kilowatts, more preferably from about 5 to about 50 kilowatts, for commercial multimode applicators.
  • the heating time generally ranges from at least about 1 second, and more generally from about 10 seconds up to about 5 minutes. At power levels of about 800-1000 watts the heating time is preferably from about 1 minute to about 2% minutes when treating single leaves as opposed to piles or stacks.
  • the range of, e.g., 2-75 kilowatts, heating times would be lower, ranging from about 5 seconds up to about 60 seconds, and generally m the 10-30 second range at, say, 50 kilowatts, again for single leaves as opposed to piles or stacks.
  • an optimal microwave field density could be determined for any given applicator based on the volume of the cavity, the power level employed, and the amount of moisture m the leaves.
  • use of higher power levels will require less time during which the leaf is subjected to the microwave radiation.
  • the microwave radiation is preferably applied to the leaf or portion thereof for a time sufficient to effectively dry the leaf, without charring, so that it is suitable for human consumption. It is also preferred to apply the microwave radiation to the leaf or portion thereof for a time and at a power level sufficient to reduce the moisture content to below about 20 % by weight, more preferably about 10% by weight.
  • a Microdry 300 kW microwave tobacco drying system 1 comprising a mobile truck frame 2 (front end at right side of drawing not shown) , a conveyo ⁇ zed microwave oven 3 which interiorly includes four modular oven cavities of single wall construction (which can be suitably constructed from 3003H14 aluminum) , each cavity measuring approximately 16' in length x 84" m width x 48" in height.
  • Each cavity is equipped with four access doors located two per side. The doors are double interlocked to prevent accidental exposure to microwave energy.
  • an automatic cutting mechanism 5 including multiple (e.g., twelve) rotating blades for removing the stem from the leaves 4.
  • the cutter can be a straight strip approximately 3.4" m width down the center of the leaves, manually fed.
  • An appropriate guard can be provided, if desired, to prevent insertion of operators' hands.
  • Figure 3 depicts a stem cutting mechanism, as noted above the whole leaves can be used m accordance with other embodiments of the invention.
  • the apparatus could employ a steam vessel or a pair of rollers for pressing moisture from the leaves .
  • the cut tobacco leaves 6 are conveyed by a belt conveyor 7 to the mam microwave oven 3 housing the four cavities.
  • the system has an oven length of approximately 78 feet.
  • the conveyor system can alternatively comprise multiple, e.g., six, variable speed polypropylene belts arranged m such a way so as to allow the cut stems to fall from between the pairs of belts and into a hopper located below the belts (not shown) .
  • the belts will then carry the cut tobacco leaves through one of two traps located one at each of the cavities, designed to contain the microwave energy, and then into a selected cavity where each leaf is subjected to microwavmg in accordance with the principles of the invention described above.
  • the conveyor carries the leaves through the cavity exit, through an oven discharge trap and out of the oven where they are then conveyed into appropriate vessels to be taken for further processing.
  • an exhaust system including suitable blowers providing recirculating air can be included m the system (see moisture exhaust vents, item 8 being one labeled as representative, m Fig. 3) .
  • the interior of tne oven can be temperature controlled by appropriately spaced circulating air convection heating sources so that the interior of the oven outside the microwave cavities is maintained at a preferred constant temperature, e.g., 160-180° F, during conveyo ⁇ zed transport of the leaves.
  • the electrical requirements can be supplied by a pair of conventional diesel -powered generators 9, 10.
  • the microwave drying system can also be operated m a fixed location, if desired, powered by conventional electrical sources.
  • Each of the four cavities withm oven 3 m Fig. 3 receives microwave energy from a corresponding Microdry Model IV-75 microwave power source.
  • the microwave energy enters each respective cavity via a splitter through two ports located m the top of each cavity.
  • a mode stirrer is located below the ports each cavity to assist m the distribution of the microwave energy.
  • Each microwave power unit is acompletely self-contained cabinet that houses the required components to operate a 75 kW magnetron. Controls for the microwave power are located on the cabinet.
  • the units are designed for unattended continuous operation in an industrial environment.
  • Each microwave power generator may be located at each cavity, or at a distance from the cavity. However, at a distance of 50' , the transmission line losses will be about 2%.
  • Each power generator provides adjustable microwave energy for industrial operation.
  • the output power is adjustable from 0 to about 75 kW at the FCC assigned frequency of 915 MHz, and is controlled by a solid state control circuit manually adjusted by a control knob on the panel or by remote control with a 4-20 milliamp control signal from a process controller. While the circuitry will control the power output from zero, the frequency spectrum becomes broad at levels below about 5 kW.
  • the power generator for each cavity is basically a direct current power supply operating an industrial magnetron which is operated and protected by circuit functions designed for automatic and manual operation. The electrical functions of the generator are monitored by meters on the control panel, located on cabinet door. The metering includes anode current, anode voltage, output power, filament current, electromagnet current and reflected power.
  • Each microwave power generator cabinet has full width doors for maximum accessibility to the components.
  • a built-m electromagnetic interference shielding enclosure houses the magnetron and associated microwave components.
  • a door allows for installation of the magnetron and electromagnet.
  • the system includes a circulator and water load, mounted inside the cabinet, which functions as an isolator to protect the magnetron in the event of a high reflected power condition.
  • the microwave power generator uses both forced air and water for cooling the heat producing components.
  • the magnetron and electromagnet are water cooled by a closed loop demmeralized water system. A separate water source and a heat exchanger can be used to cool the water m this loop.
  • the separate water source also flows through a water to air heat exchanger inside the cabinet to cool the cabinet air.
  • a high pressure centrifugal blower provides cooling to the magnetron output window and the cathode structure. Water and cabinet temperatures are interlocked in the control power chain.
  • Typical reference data for each microwave generator in a system of this are as follows: Power input 95 KVA, 440-480 VAC, 3 phase, 60 Hz
  • Magnetron tube CTL, CWM 75 I Typical magnetron operation reference data are as follows:
  • a typical microwave generator can employ a carbon steel enclosure and have an output connection (WR 975 waveguide) m the top of the cabinet at an appropriate location.
  • a microwave tobacco drying system generally designed as described above was effective to eliminate over 80% of the moisture content of the leaves.
  • m one measured sample 15 pounds of leaves with an assumed initial water content of 85 wt% and solids content of 15 wt% was conveyed through a microwave cavity m single leaf thickness at a rate of about 180 lbs per hour.
  • the leaves were weighed after exiting the cavity.
  • the ending weight was 4.6 lbs., or 31% of the initial weight.
  • therer remained 2.35 pounds of water m the leaves, corresponding to 18.5% of the initial water content.
  • the microwave treatment of yellow tobacco m accordance with the present invention preferably results m a dried, golden-colored tobacco product.
  • the data presented herein establish that such dried tobacco, m its unsmoked form, has dramatically reduced carcinogenic nitrosamines, particularly NNN and NNK, as opposed to normally cured tobacco.
  • concentrated forms of electromagnetic radiation i.e., concentrated as distinguished from general exposure to sunlight or electric light withm the visible spectrum
  • TSNAs m tobacco products can be used to achieve the basic objects of the present invention - reduction or substantial elimination of TSNAs m tobacco products, by treating the tobacco with such energy forms m approximately the same time frame post -harvest as discussed above with regard to the microwave embodiment.
  • the same general and preferred techniques and principles discussed above regarding microwavmg can be applied when such an alternate energy source is used; for example, the tobacco is treated with such radiation at approximately the same time frames post- harvest, the leaves can be de-stemmed, pressed between rollers or steamed prior to irradiation, etc.
  • any electromagnetic radiation source, and accelerated particle beams such as electron beams, having frequencies higher than the microwave domain with the conventional electromagnetic spectrum are operative to significantly reduce, substantially eliminate and/or prevent formation of TSNAs when tobacco is uncured and m a state susceptible to having the amount of TSNAs reduced or formation thereof arrested.
  • microwaves are generally defined as inclusive of those forms of electromagnetic radiation having a frequency of 10 11 Hz and a wavelength of 3 x 10 3 meters
  • energy sources include, without limitation, far-infrared and infrared radiation having frequencies of about 10 12 to 10 14 Hz and wavelengths of 3 x 10 4 to 3 x 10 "6 meters, ultraviolet radiation having frequencies of about 10 16 to 10 18 Hz and wavelengths of 3 x 10 8 to 3 x 10 "10 meters, soft x-rays or lasers, cathode rays (a stream of negatively charged electrons issuing from the cathode of a vacuum tube perpendicular to the surface) , x-rays and gamma radiation typically characterized as having frequencies of 10 21 Hz and higher at corresponding wavelengths .
  • radiation application times of less than one minute, preferably less than 30 seconds and even more preferably less than about ten seconds are needed when using such higher frequency radiation sources.
  • radiation application times of at least about one second are preferred.
  • the exposure rate can be controlled to deliver the radiation dosage over time, if desired.
  • 1 megarad of radiation can be delivered instantaneously (as with the electron beam accelerator discussed below m Example 17) , or at a predetermined exposure rate (as exemplified by the closed chamber gamma irradiation testing discussed below m Example 19, wherein 1 megarad (10 kGrey) of irradiation was delivered at an exposure rate of about .8 megarad per hour) .
  • a predetermined exposure rate as exemplified by the closed chamber gamma irradiation testing discussed below m Example 19, wherein 1 megarad (10 kGrey) of irradiation was delivered at an exposure rate of about .8 megarad per hour.
  • the particular radiation dosages and exposure rate will depend on the particular equipment and type of radiation source being applied, as would be apparent to one of ordinary skill in the art, it is generally preferred to subject the tobacco samples to radiation of from about .1 to about 10 megarads, more preferably from about .5 to about 5 megarads, and more preferably from about .75 to about 1.5 megarads.
  • a recirculating air convection oven has also been demonstrated to reduce the TSNA content, albeit with reduced leaf quality.
  • heating in a recirculating air convection oven at temperatures of from about 100° to about 500° F, for periods ranging from one hour at the low end down to about 5 minutes at the high end of the temperature scale can also effectively reduce the content of or arrest formation of TSNAs m tobacco while m its susceptible state as defined herein.
  • an oven combining recirculating air convection heat and microwave radiation can shorten the heating time while providing improved quality to the leaves.
  • the present invention relates to a method for reducing or substantially eliminating the content of tobacco- specific nitrosamines m a human or animal subject who smokes, chews or otherwise ingests tobacco, by providing for consumption a tobacco product having significantly reduced or substantially eliminated TSNAs.
  • the improved tobacco of the present invention can be substituted m whole or part for normally-cured tobacco m any tobacco product, including cigarettes, cigars, chewing tobacco, tobacco chewing gum, tobacco lozenges, tobacco pouches, snuff, or tobacco flavoring and food additives.
  • the present invention provides a less noxious odor while maintaining good smoking characteristics and providing full flavor with normal nicotine content.
  • the tobacco of the present invention has a rich, pleasant flavor.
  • Example 1 Virginia flue tobacco was harvested, and the leaves were placed m a curing barn at about 100-110°F to begin the flue- curmg process. Samples 1-3 were taken from the barn after the leaves had turned yellow, about 24-36 hours post-harvest. Sample 1 was a lamina sample, stripped of the midrib, and baked m a convection air oven at about 400-500°C for about 1 hour, which browned the lamina. Sample 2 was a yellow leaf, placed m a Goldstar Model MA-1572M microwave oven (2450 MHz) , and heated on the high power setting (1,000 watts) while rotating for about 2% minutes. Sample 3 was a yellow leaf, untreated, used as a control . Samples 4 and 5 remained m the curing barn under elevated temperature of about 180°F, Sample 4 being dried outside the racks and Sample 5 inside the racks. Sample 6 was a cured, brown leaf, having underwent the normal flue-cure process.
  • TSNA represents the sum of these four tobacco-specific nitrosamines.
  • Sample work-up and extraction followed a typical procedure for analysis of TSNAs (see, for example, Burton et al . , "Distribution of Tobacco Constituents m Tobacco Leaf Tissue. 1. Tobacco-specific Nitrosamines, Nitrate, Nitrite and Alkaloids", J. Agric. Food Chem., Volume 40, No. 6, 1992), and individual TSNAs were quantified on a Thermedics Inc.
  • Example 2 Virginia flue tobacco was harvested. Sample 7 was a fresh- cut, green leaf used as a control, while Sample 8 was a fresh-cut green leaf which was subjected to microwave radiation m a multimode microwave applicator manufactured ioy MicroDry of Louisville, Kentucky, operating at 2450 MHz at 2.5 kilowatts, for about 20 seconds. Samples 9-12 were made from normally flue- cured brown tobacco. Sample 9 was tobacco from a formed cigarette; Sample 10 was loose, shredded tobacco for making cigarettes; Samples 11 and 12 were the same as Samples 9 (cigarette) and 10 (loose) , respectively, except that each was subjected to the same microwave conditions as Sample 8. TSNA contents were analyzed m the same manner as m Example 1. The results are shown m Table 2 below: Table 2
  • Example 3 The following cigarette brands shown in Table 3 were purchased at random at various retailers in Lexington, Kentucky, and analyzed for TSNA content using the procedure described in Example 1 :
  • Example 4 Virginia flue tobacco was harvested, and the leaves were placed in a curing barn at about 100-110°F to begin the flue- curing process. After the leaves turned yellow, about 24-36 hours post -harvest , they were taken out of the barn and microwaved in Goldstar Model MA-1572M microwave oven (2450 MHz) , high power setting (1000 watts) , for about 24 minutes while rotating. The leaves were effectively dried by this procedure, although they did not turn brown, but instead retained their golden-yellow color. The leaves were shredded and made into cigarettes. Samples 29-33 were taken from a batch labeled Red Full Flavor, while Samples 34-38 were taken from a batch labeled blue Light. Samples 39-42 were cigarettes purchased at a health food store, under the brand Natural American Spirit. Samples 29- 42 were analyzed for TSNA content using the procedure described in Example 1, and the results are shown in Table 4 below:
  • Example 5 Virginia flue tobacco was harvested, and the leaves were placed in a curing barn at about 100-110°F to begin the flue- curing process.
  • Samples 43-44 were taken from the barn after the leaves had turned yellow, about 24-36 hours post -harvest , and subjected to microwave radiation in the MicroDry multimode applicator described above for about 20 and 30 seconds, respectively, at a power level of about 6 kilowatts.
  • Samples 43 and 44 were dried, golden-yellow leaves after the microwaving.
  • Samples 45-51 were made from brown, cured leaves having underwent the normal flue-cure process.
  • Sample 45 was a control; Samples 46 and 47 were baked in a convection oven preheated to about 400- 500 °F for about 1 and about 3 minutes, respectively; and Samples 48 and 49 were subjected to microwave radiation (915 MHz) in a Waveguide applicator Model WR-975, a large multimode oven manufactured by MicroDry (power settings from 0 - 75 KW) at 50 kilowatts for about 10 and 40 seconds, respectively. Samples 50 and 51 were cut (reconstituted sheet) tobacco made from the flue- cured leaves.
  • Sample 50 was subjected to microwave radiation in the Waveguide microwave oven at 50 kilowatts for about 1.5 minutes, while Sample 51 was baked in a convection oven preheated to about 400-500 °F for about 3 minutes. These samples were analyzed for TSNA content using the procedure described in Example 1, and the results are shown in Table 5 below:
  • Example 6 Virginia flue tobacco was harvested, and the leaves were placed in a curing bar at about 100-110°F to begin the flue- curing process.
  • Samples 52-55 were cigarettes made from yellow tobacco which had been pulled from the barn after about 24-36 hours, and subjected to Microwave radiation m a Goldstar microwave oven, Model MA-1572M (2450 MHz) , for about 2 minutes on the high power setting (1000 watts) .
  • Samples 61 and 62 were cigarettes made from leaves which had undergone the normal flue-cure process, without microwave treatment.
  • Sample 56 was a cured leaf;
  • Sample 57 was post-yellow, not fully cured;
  • Sample 58 was a cured lamina, while Samples 59 and 60 were cured midribs.
  • TSNA contents were measured as in Example 1, and the results are set forth in Table 6 below:
  • Example 7 Virginia flue tobacco was harvested. Samples 63 and 66 were uncured, fresh-cut green tobacco, although over a week lapsed before TSNA measurements were taken, so some air-curing had taken place. The remaining leaves were placed in a curing barn at about 100-110°F to begin the flue-curing process. Sample 68 was a leaf taken from the barn after it had turned yellow, about 24- 36 hours post-harvest, and was subjected to microwave radiation m the Waveguide multimode applicator described above, for about 40 seconds at 25 kilowatts.
  • Samples 64/65 (leaves) and 67/70 demonstrate the effects of the present invention when cured tobacco is rehydrated, then subjected to microwave radiation.
  • Samples 64 and 65 were leaf samples having undergone the normal flue-curing process; however, Sample 64 was rehydrated by running under an open faucet for about 5-10 seconds. The leaf absorbed significant moisture.
  • Each of Samples 64 and 65 was then microwaved m the Waveguide multimode applicator for about 40 seconds at 25 kilowatts.
  • Samples 67 and 70 were reconstituted sheet tobacco samples, made from cured leaves. Sample 67 was rehydrated by adding water so that a significant quantity was absorbed, then microwaved under the conditions described for Sample 64. Sample 70 was not microwaved.
  • Samples 69, 71 and 72 are additional cured leaf samples, used as controls.
  • the TSNA contents were measured as in Example 1, and the results are shown m Table 7 below:
  • Example 8 Virginia flue tobacco was harvested, and the leaves were placed in a curing barn at about 100-110° F to begin the flue- curing process.
  • Sample 73 was a leaf taken from the barn after it turned yellow, about 24-36 hours post-harvest, and microwaved in a Goldstar Model MA-1572M for about 2 minutes on the high setting.
  • Samples 74-76 were flue-cured in the normal way.
  • Sample 74 was a cured control.
  • Samples 75 and 76 were rehydrated as in Example 7 (Sample 64) , then each sample was subjected to microwave radiation in the MicroDry applicator (2450 MHz) for about 20 seconds (Sample 75) and about 40 seconds (Sample 76) , respectively, at power levels of about 6 kilowatts. Samples 77- 79 were reconstituted sheet tobacco, made from the flue-cured leaves. Sample 77 was a control, while Samples 78 and 79 were rehydrated as in Example 7 (Sample 67) .
  • Samples 78 and 79 were microwaved in the MicroDry applicator for about 30 seconds each; Sample 78 rested on the oven bottom, while Sample 79 was raised up several inches by resting the sheet sample on a styrofoam cup, which permitted more uniform heating.
  • TSNA contents were measured as m Example 1, and the results are set forth in Table 8 below:
  • Samples 80-81 were Redman chewing tobacco purchased at retail. Sample 80 was a control, while Sample 81 was microwaved in a Goldstar Model MA-1572M for about 1-2 minutes on the high power setting. Samples 82-83 were Skoal snuff purchased at retail. Sample 82 was a control, while Sample 83 was microwaved in the same manner as for Sample 81. TSNA contents were measured, and the results are shown in Table 9 below:
  • Example 10 To test whether TSNAs accumulate over time even after yellow tobacco is microwaved in accordance with the present invention, additional samples (designated -A) of the cigarettes tested in Example 4, Samples 29, 35 and 39 (control) were retested for TSNA content more than seven months after the TSNA contents were first measured, as reported in Example 4. The results are shown below in Table 10 : Table 10
  • Example 11 Virginia flue tobacco was harvested, and the leaves were placed in a curing barn at about 100-110°F to begin the flue- curing process. After the leaves turned yellow, about 24-36 hours post- harvest, they were taken from the barn and subjected to microwave radiation in a Goldstar Model MA-1572M microwave oven for about 2 to 2% minutes, on the high power setting. Each of the leaves was a golden-yellow color, and effectively dried. Certain samples, designated by "ground”, were later ground up into a flour-like substance, which would be useful as, for example, a gum, lozenge or food additive. After more than six months from the time the leaves were microwaved, the TSNA content of the following samples were measured using the procedure described in Example 1. The results are shown Table 11 below: Table 11
  • Example 12 Virginia flue tobacco was harvested, and the leaves were placed in a curing barn at about 100-110°F to begin the flue- curing process.
  • Samples 104 and 105 were leaf samples having undergone the normal flue-curing process, without microwave treatment. Sample 104 was a cured midrib, while Sample 105 was cured a lamina.
  • Sample 106 was yellow tobacco, taken from the barn after the leaves had turned yellow, about 24-36 hours post harvest. After being taken from the barn, the leaves were subjected to microwave radiation in a Goldstar Model MA-1572M microwave oven for about 2-2 minutes, on the high power setting. Each of the leaves was a golden-yellow color, and effectively dried. Certain of the dried leaves were further processed in a conventional manner to form a tobacco extract, which was designated Sample 107 for purposes of analysis.
  • the TSNA contents of Samples 104-107 were measured using the procedure described in Example 1. The results are shown in Table 12 below.
  • Example 13 Virginia flue tobacco was harvested, and the leaves were placed in a curing barn at about 100-110°F to begin the flue- curing process.
  • Samples 108 and 109 were leaf samples having undergone the normal flue-curing process.
  • Sample 108 was a cured lamina, while sample 109 was a cured midrib.
  • Samples 110 and 111 were yellow tobacco, taken from the barn after the leaves had turned yellow, about 24-36 hours post-harvest. After being taken from the barn, Samples 110 and 111 were heated in a circulating air convection oven, a Sharp Carousel Convection/Microwave Model No. R-9H84B. Sample 110 was rapidly heated at about 300°F for between 5-10 minutes.
  • Sample 111 was more slowly heated at lower temperatures, starting at about 100°F and being stepped up to about 150°F after more than 10 minutes, for a total heating time of over 20 minutes.
  • the TSNA contents of Samples 108-111 were measured using the procedure described in Example 1. The results are shown in Table 13 below. Table 13
  • the convection oven heating was shown to reduce TSNA levels, the quality of the tobacco was inferior to that obtained upon microwavmg m accordance with preferred examples of the invention.
  • the heating time is necessarily longer than when using the microwave radiation treatment or other forms of higher frequency radiation.
  • the convection heating was unable to lock the color in at the desired golden- yellow, and the lamma had a tendency to be over-dried and therefore brittle, while the veins and midrib were not completely dried.
  • the microwaved leaves were effectively dried and retained a golden-yellow color after being subjected to treatment, while staying supple and pliable for further processing, especially as cigarettes.
  • Example 14 Kentucky burley tobacco was harvested, and the leaves were processed as follows after they began to turn yellow, about 24-48 hours post-harvest. Samples 112-117 were leaf samples from this batch, further processed as follows. Sample 112 was microwaved under approximately the same conditions as Sample 106 m Example 12. The leaves were a golden-yellow color and effectively dried. Samples 113, and 114 and 117 were heated m the same circulating air convection oven as described m Example 13, Sample 113 being heated under approximately the same conditions as Sample 110, Sample 114 being heated under approximately the same conditions as Sample 111, and Sample 117 being heated at about 350°F for about 20 minutes.
  • Samples 113, 114 and 117 were akin to that of Samples 110 and 111, as described m Example 13.
  • Samples 115 and 116 were heated m the Sharp Carousel Convection/Microwave oven described m Example 13, using the combined microwave (30%) /convection (300°C) feature until the leaves were effectively dried to golden-yellow color.
  • the TSNA contents of Samples 112-117 were measured using the procedure described m Example 1. The results are shown m Table 14 below:
  • Example 15 Virginia flue tobacco was harvested, and the leaves were placed m a curing barn at about 100-110°F to begin the flue- curmg process.
  • Samples 118-120 were leaf samples, taken from the barn after the onset of yellowing, and shortly thereafter subjected to microwave radiation in a conventional kitchen-type microwave oven for about 2 to 2 1/2 minutes until the leaves were effectively dried to a golden-yellow color, without burning or charring.
  • Samples 121-123 were samples of Kentucky burley tobacco, harvested and processed after the onset of yellowing m each instance as follows. Sample 121 was placed m a conventional steam tumble dryer typically used m the tobacco industry, at a temperature of about 200°F, until the leaves had browned and dried somewhat.
  • Sample 122 was microwaved m the above-referenced Goldstar microwave on high for about 2 minutes, the rehydrated with water and placed in the tumble dryer to impart a slight browning to the leaves which is believed to enhance the flavor.
  • Sample 123 was treated like Sample 122, except that it was microwaved for 1 minute and was not rehydrated before being put in the tumble dryer.
  • TSNA contents were likewise measured as in Example 1, and the results are shown in Table 15 below:
  • Example 16 North Carolina burley tobacco was harvested, and the leaves were processed as follows after they began to turn yellow, about 2-3 days post -harvest .
  • Sample 118 was a leaf sample which had been subjected to microwave radiation in the same type of Goldstar microwave oven described above, on the high power setting for about 2 minutes. After microwaving the leaves were a golden yellow color, and effectively dried.
  • the TSNA content was measured using the procedure described m Example 1. The results are shown m Table 16 below:
  • Example 17 This example demonstrates the effectiveness of using electron beam radiation to reduce the content of, or substantially prevent formation of TSNAs, yellow tobacco samples.
  • North Carolina burley tobacco was harvested.
  • Samples 119-122 were leaf samples, air-cured by hanging outside in a normal manner, until the leaves were effectively dried and brown. Sample 119 was untreated as a control.
  • Samples 120 and 121 were subjected to electron beam radiation on a conveyor belt using a Dynamitron Electron Beam Accelerator, manufactured by Radiation Dynamics, Inc. of Edgewood, N.Y., at an exposure rate of 1 megerad.
  • Sample 122 was subjected to microwave radiation m the Goldstar microwave oven for about 2 minutes on the high power setting.
  • Sample 123 was taken from the tip of a burley leaf after it had begun to turn yellow.
  • Sample 124 was a leaf stem portion, taken from the same plant as Sample 123, and was still somewhat green-colored.
  • Samples 125 and 126 were whole leaf burley samples, at the yellow stage.
  • Each of Samples 123-126 was subjected to electron beam radiation using the aoove-descnbmg Dynamitron, the same manner and under the same exposure rate as Samples 120 and 121, as described above. The above samples were tested to measure TSNA content according to the procedure set forth m Example 1, and the results are shown m Table 17 below:
  • Example 18 This example demonstrates that high energy beams produced by lasers are also effective to achieve the low TSNA goals of the present invention.
  • a NovaScan handpiece was used under the superpulse E program, which determines the speed of application in patterns per second.
  • a setting of E10 was used, which delivers 10 patterns per second.
  • T-l - - 1 pass each side T-5 • - 1 pass each side
  • T-2 - - 2 passes each side
  • T-6 - - 2 passes each side
  • T-3 - - 3 passes each side
  • T-7 - - 3 passes each side
  • T-4 - - 4 passes each side
  • T-8 - - 4 passes each side
  • the C0 2 laser irradiated samples were not dried as effectively as the microwaved samples, although the TSNA contents were low, and therefore an additional drying step could be employed to speed the curing process. Also, after the C0 2 laser irradiation but prior to TSNA testing, six of the eight subsamples turned somewhat brown, with no apparent effect on TSNA content.
  • Example 19 This example demonstrates that gamma radiation is also effective in preventing formation of significant amounts of TSNA in yellow tobacco.
  • Virginia flue tobacco was taken about 2-3 days post harvest, ust after the leaves had turned yellow.
  • Each of Samples 129-132 was taken from the lamma portion of the yellow leaves, and subjected m an enclosed chamber to gamma irradiation of 10 kGrey (1 megarad) at an exposure rate of 8 kGrey (.8 megarad) per hour, for a total exposure time of about 75 minutes.
  • the irradiated samples were subsequently evaluated as to TSNA content m the same fashion as described above, and the results are shown below m Table 19: Tabl e 19

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  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
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Abstract

L'invention concerne des procédés visant à réduire la teneur en nitrosamines cancérigènes dans certains végétaux à feuilles cultivés (par exemple, tabac et marijuana) et à empêcher la formation de ces substances, lesdits procédés consistant à soumettre les feuilles récoltées à des rayonnements en hyperfréquences et/ou aux fréquences plus élevées, à des stades appropriés du cycle de traitement. S'agissant du tabac, on peut fabriquer des produits convenant à la consommation humaine (cigarettes, cigares, etc.) grâce aux procédés décrits, ce qui donne dans les produits résultants une teneur en nitrosamines spécifiques du tabac qui équivaut à la teneur propre au tabac vert fraîchement coupé. Dans les modes de réalisation préférés, les produits résultants sont séchés, et les feuilles de tabac jaune doré ont alors une teneur presque négligeable en substances cancérigènes connues, NNN et NNK, par rapport au tabac traité de manière classique.
EP98929002A 1997-06-20 1998-06-09 Procedes de traitement du tabac visant a reduire la teneur en nitrosamines, et produits resultants Withdrawn EP0991329A4 (fr)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
US08/879,905 US6135121A (en) 1996-06-28 1997-06-20 Tobacco products having reduced nitrosamine content
US879905 1997-06-20
US99804397A 1997-12-23 1997-12-23
US998043 1997-12-23
PCT/US1998/012128 WO1998058555A1 (fr) 1997-06-20 1998-06-09 Procedes de traitement du tabac visant a reduire la teneur en nitrosamines, et produits resultants

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EP0991329A1 true EP0991329A1 (fr) 2000-04-12
EP0991329A4 EP0991329A4 (fr) 2006-06-14

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HUP0002532A3 (en) 2001-03-28
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CA2294130C (fr) 2006-09-05
GEP20022696B (en) 2002-05-27
IL154166A0 (en) 2003-07-31
EA002448B1 (ru) 2002-04-25
GEP20033111B (en) 2003-11-25
EE9900590A (et) 2000-08-15
WO1998058555A1 (fr) 1998-12-30
TR200200658T2 (tr) 2002-09-23
JP2002503965A (ja) 2002-02-05
IL154166A (en) 2005-09-25
KR100458405B1 (ko) 2004-11-26
PL188860B1 (pl) 2005-05-31
NO312325B1 (no) 2002-04-29
JP3996958B2 (ja) 2007-10-24
TR199903160T2 (xx) 2000-10-23
CN1272768A (zh) 2000-11-08
KR20010014034A (ko) 2001-02-26
IL133583A0 (en) 2001-04-30
EA200000053A1 (ru) 2000-08-28
YU68799A (sh) 2001-05-28
AU8067098A (en) 1999-01-04
IL133583A (en) 2003-06-24
OA11240A (en) 2003-05-30
BR9810060A (pt) 2002-07-16
OA11738A (en) 2005-05-13
AP1524A (en) 2005-12-22
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