CN104284605A

CN104284605A - Method for treating an extracted tobacco pulp and tobacco products made therefrom

Info

Publication number: CN104284605A
Application number: CN201380025350.7A
Authority: CN
Inventors: C·D·H·伯德; 浦彦; A·R·杰拉尔迪; C·B·小罗兹
Original assignee: RJ Reynolds Tobacco Co
Current assignee: RJ Reynolds Tobacco Co
Priority date: 2012-03-19
Filing date: 2013-03-19
Publication date: 2015-01-14
Anticipated expiration: 2033-03-19
Also published as: JP6255379B2; EP2827727B1; EP2827727A1; WO2013142483A1; CN104284605B; JP2015510777A

Abstract

The invention provides a method of producing a tobacco composition for use in a tobacco product, the method including treating a tobacco pulp with supercritical carbon dioxide. The treated tobacco pulp may exhibit a benzo[a]pyrene concentration lower than the initial benzo[a]pyrene concentration and/or a TSNA concentration lower than the initial TSNA concentration. The treated pulp can be introduced into tobacco products including smoking articles, smokeless tobacco products, and aerosol-generating devices configured for non-combustion of plant materials.

Description

For the treatment of method and the tobacco product prepared thus of the tobacco pulp extracted

Technical field

Present disclosure relates to the product made from tobacco or derive, or otherwise comprises tobacco and be intended for the product of human consumption.Particularly, present disclosure relates to the composition or preparation that comprise tobacco, be such as intended to use with smokeless form those.

Background technology

Cigarette, cigar and pipe tobacco are the common smoking products being in multi-form use tobacco.These smoking products of following use: heating or burning tobacco, to produce the aerosol (as cigarette) that can be sucked by smoker.Tobacco can also be enjoyed with so-called " smokelessly " form.By inserting in user's mouth by the treated tobacco of some forms or containing tobacco formulation, use smokeless tobacco product popular especially.See such as, the U.S. Patent number 1,376,586 of smokeless tobacco preparation type, composition and the processing method set forth in following document: Schwartz; The U.S. Patent number 3,696,917 of Levi; The U.S. Patent number 4,513,756 of the people such as Pittman; The U.S. Patent number 4,528,993 of the people such as Sensabaugh, Jr.; The U.S. Patent number 4,624,269 of the people such as Story; The U.S. Patent number 4,991,599 of Tibbetts; The U.S. Patent number 4,987,907 of Townsend; The U.S. Patent number 5,092,352 of the people such as Sprinkle, III; The U.S. Patent number 5,387,416 of the people such as White; The U.S. Patent number 6,668,839 of Williams; The U.S. Patent number 6,834,654 of Williams; The U.S. Patent number 6,953,040 of the people such as Atchley; The U.S. Patent number 7,032,601 of the people such as Atchley; With the U.S. Patent number 7,694,686 of the people such as Breslin; The U.S. Patent Publication No. 2004/0020503 of Williams; The U.S. Patent Publication No. 2005/0115580 of the people such as Quinter; The U.S. Patent Publication No. 2005/0244521 of the people such as Strickland; The U.S. Patent Publication No. 2006/0191548 of the people such as Strickland; The U.S. Patent Publication No. 2007/0062549 of the people such as Holton, Jr.; The U.S. Patent Publication No. 2007/0186941 of the people such as Holton, Jr.; The U.S. Patent Publication No. 2007/0186942 of the people such as Strickland; The U.S. Patent Publication No. 2008/0029110 of the people such as Dube; The U.S. Patent Publication No. 2008/0029116 of the people such as Robinson; The U.S. Patent Publication No. 2008/0029117 of the people such as Mua; The U.S. Patent Publication No. 2008/0173317 of the people such as Robinson; The U.S. Patent Publication No. 2008/0196730 of the people such as Engstrom; The U.S. Patent Publication No. 2008/0209586 of the people such as Neilsen; The U.S. Patent Publication No. 2008/0305216 of the people such as Crawford; The U.S. Patent Publication No. 2009/0065013 of the people such as Essen; With the U.S. Patent Publication No. 2009/0293889 of the people such as Kumar; The PCT WO 04/095959 of the people such as Arnarp; With the U.S. Patent Application Serial 12/638,394 of the people such as Mua submitted on December 15th, 2009; Each section in them is incorporated to herein by reference.

One class smokeless tobacco product is referred to as " snuff ".In US and European, the representative type (being commonly referred to as " snus ") particularly manufacturing moist snuff product in Sweden.See, such as, the people such as Bryzgalov, 1N1800 Life Cycle Assessment, Comparative Life Cycle Assessment of General Loose and Portion Snus (2005).In addition, manufacture some relevant quality standard with snus and be combined into so-called GothiaTek standard.Exemplary smokeless tobacco product comprises: CAMEL Snus, the CAMEL Orbs of R.J.Reynolds Tobacco Company, CAMEL Strips and CAMEL Sticks; The REVEL Mint Tobacco Packs of U.S.Smokeless Tobacco Company and SKOAL Snus; And MARLBORO Snus and Taboka of Philip Morris USA.

Various processing method and additive are proposed, for changing overall characteristic or the character of the tobacco-containing material used in tobacco product.Such as, use additive or processing method, to change chemistry or the organoleptic properties of tobacco-containing material, or when the tobacco-containing material that can aspirate, change chemistry or the organoleptic properties of the main flume produced by the smoking product comprising tobacco-containing material.See, such as, the people such as Leffingwell, Tobacco Flavoring for Smoking Products, R.J.Reynolds Tobacco Company (1972), it is incorporated to herein by reference.In addition, processed in a specific way or fusion tobacco-containing material, described mode is designed to realize certain sensation or chemical characteristic.See, such as, the U.S. Patent Publication No. 2008/0245377 of the people such as the U.S. Patent number 7,025,066 of the people such as Lawson and Marshall, they are incorporated to herein by reference.

Desirable to provide a kind of tobacco product such as smokeless tobacco product of pleasant form, and provide the method containing tobacco compositions prepared and be applicable in smokeless tobacco product.

Summary of the invention

The present invention relates to a kind of tobacco product, such as be intended to or be configured for and insert smokeless tobacco product in user mouth (such as, moist snuff, dry snuff, chewing tobacco, containing the chewing gum of tobacco and the soluble tobacco product that maybe can melt), also relate to the method that preparation is suitable for the preparation in such tobacco product.Tobacco product of the present invention comprises good to eat tobacco compositions, such as has the composition of the form of extract that to toast tobacco through fire.In one embodiment, the invention provides and to toast tobacco extract through fire, its show with the special sense characteristic toasting tobacco relevant through fire (such as, cigarette fragrance or fragrance), also show chemical composition difference, the benzo such as reduced [a] pyrene or other polycyclic aromatic hydrocarbon level favourable compared with the toasting tobacco through fire of complete form simultaneously.

Described extract normally through the aqueous extract of baking tobacco-containing material, but can use the proton solvent of some other polarity or comprise the cosolvent mixture of water, and does not depart from the present invention.The concentration of benzo [a] pyrene in described extract is no more than about 10ppb usually, is often no more than about 5ppb.

Although smokeless tobacco composition is by the tobacco product type of the particular importance of being benefited from extract of the present invention, other tobacco product also can be benefited from so good to eat tobacco compositions, such as smoking product (such as, cigarette) or produce aerocolloidal device, described device contains tobacco or tobacco ingredient, but not burning tobacco or other vegetable material.Usually, described tobacco product comprises tobacco-containing material or the non-tobacco vegetable material carrier as described extract.

In another embodiment, use extract of the present invention to form the tobacco-containing material of reconstruct.Particularly, such material can comprise with through the tobacco pulp that extracts (such as, through fiery flue-cured tobacco straw pulp) combined extract of the present invention (such as, toasting tobacco extract through fire), wherein said slurry through pretreatment to reduce benzo [a] pyrene concentration.Such as, can by supercritical carbon dioxide extract pretreatment through extraction through fiery flue-cured tobacco straw pulp, thus reduce benzo [a] pyrene concentration.

In yet another aspect, the invention provides a kind of method of producing good to eat tobacco compositions, the feature of described tobacco compositions is benzo [a] the pyrene concentration of the sense quality relevant with the material that toasts tobacco through fire and reduction.Described method comprises the steps: to have the first benzo [a] pyrene concentration (such as, at least about 100ppb benzo [a] pyrene) toast tobacco material and polar aprotic solvent (such as through fire, water or comprise the cosolvent mixture of water) mixing is to produce slurry, described slurry can provide the described intimate contact toasted tobacco between material and described polar aprotic solvent through fire.Described method also comprises: be enough to maintain the time being enough to form extract at the temperature forming extract by described slurry, described extract comprises the component dissolved in described polar aprotic solvent through baking tobacco-containing material, described extract shows the second benzo [a] the pyrene concentration (such as, being less than about 10ppb benzo [a] pyrene) lower than described first benzo [a] pyrene concentration.After this, described extract is separated with remaining pulp material, described remaining pulp material comprises and is insoluble to toasting tobacco material component through fire of described polar aprotic solvent.Described method also comprises the steps: to utilize described extract as good to eat tobacco compositions usually; such as; by the extract of described separation is introduced in tobacco product; this often comprises: the extract of described separation is applied to tobacco-containing material or non-tobacco vegetable material; to form treated material, then can be mixed in tobacco product.In certain embodiments, after slurry process, described extract and the slurry through extracting are recombinated, to reduce benzo [a] pyrene content, the second extraction of such as starching can remove benzo [a] pyrene.Such as, described method can comprise: with the remaining pulp material of supercritical carbon dioxide treatment, to reduce benzo [a] pyrene concentration and to form the pulp material with benzo [a] the pyrene concentration of reduction, after this extract of described separation is applied to the pulp material of benzo [a] the pyrene concentration with reduction, to form treated material.If necessary, before mixing in tobacco product, by removing solvent at least partially, described extract can be concentrated.

In one particular embodiment, the invention provides a kind of method of composition for the preparation of being suitable as smokeless tobacco composition, described method comprises: will have the mixing with water starch to produce water-based through the fire material that toasts tobacco of the first benzo [a] pyrene concentration, described slurry can provide the described intimate contact toasted tobacco between material and described water through fire; By described slurry be enough to be formed through fire toast tobacco extract temperature under maintain the time being enough to form the extract that to toast tobacco through fire, describedly comprise the component of to toast tobacco through fire the water-soluble good to eat of material and aromatics through the fire extract that toasts tobacco, described water-based shows the second benzo [a] pyrene concentration lower than described first benzo [a] pyrene concentration through the fire extract that toasts tobacco; Described water-based is separated with remaining pulp material through the fire extract that toasts tobacco, and described remaining pulp material comprises and water-fastly to toast tobacco material component through fire; Mix with tobacco or non-tobacco vegetable material, to form smokeless tobacco composition through the fire extract that toasts tobacco with by described water-based.

Accompanying drawing explanation

In order to provide the understanding to embodiment of the present invention, with reference to accompanying drawing, described accompanying drawing is not necessarily drawn in proportion, and wherein Reference numeral represents the component of exemplary of the present invention.Accompanying drawing is only exemplary, should not be construed as restriction the present invention.

Fig. 1 is the decomposition diagram of the smoking product with cigarette form, which show the smokeable material of cigarette, packaging material parts and filter element; With

Fig. 2 is the viewgraph of cross-section of smokeless tobacco product embodiment, and its width along product is made, and shows the outer pouch being filled with smokeless tobacco composition of the present invention.

Detailed description of the invention

More fully the present invention will be described hereinafter now.But the present invention can specialize in many different forms, should not be construed as the embodiment being limited to and setting forth herein; On the contrary, provide these embodiments to be to make present disclosure thoroughly with complete, and fully pass on scope of the present invention to those skilled in the art.As in the present description and claims use, singulative " ", " one " and " described " comprise plural referents, unless the context clearly indicates otherwise.The weight represented based on dry ingredient (that is, all the components) is in addition to water mentioned to " dry weight percentage " or " based on dry weight ".

The invention provides a kind of method of the good to eat tobacco compositions for the preparation of tobacco extract form.In certain embodiments, extract of the present invention provides a kind of tobacco compositions, and it has some compound be present in undrawn tobacco-containing material of the amount of favourable sense quality and minimizing.Method of the present invention is specially adapted to the extract forming the material that to toast tobacco through fire, although it can be applied to other tobacco-containing material, such as uses the tobacco of other baking tech baking (tobacco-containing material that is that such as, dry and/or flue baking).See, such as, the technology for baking tobacco set forth in the U.S. Patent Application Publication No. 2012/0037175 and the selected bibliography wherein quoted of the people such as Cantrell, they by reference entirety be incorporated to.

" toasting tobacco through fire " used herein represents the tobacco-containing material carrying out fiery curing process.In fire is roasting, tobacco leaf is exposed to the combustion product of the naked light of hanging oneself in baking shell, usual continued for several weeks, thus produces special cigarette fragrance and fragrance.In some cases, that the special sense characteristic toasted tobacco through fire can also be described as is woody flavour, sweet, that have nut taste, fragrance, have native taste or tart flavour.That fire for such baking technique is characterized as being low combustion usually or glow, this means, described fire is maintained at the state promoting that cigarette produces.Toast tobacco through fire and be sometimes referred to as " dark color toasts tobacco through fire ".See, such as, the fiery curing process of setting forth in the U.S. Patent number 7,650,891 of the people such as Groves and the U.S. Patent number 7,757,697 of the people such as U.S. Patent number 7,650,892 and Thomas and the tobacco character obtained, they are incorporated to herein all by reference.Also see, Tobacco Production, Chemistry and Technology, the 164-182 page of the people such as Davis (volume) (1999).

In the roasted journey of fire, tobacco-containing material involve in the intimate interaction of the combustion product of the fire in baking shell with contact, this means, the surface of the direct Exposure To Tobacco material of the cigarette from fire.This interaction between cigarette and tobacco can cause the chemical change of tobacco-containing material, and described chemical change causes usually with other chemical change of not too wishing in the special cigarette fragrance toasted tobacco through fire and fragrance and tobacco.The invention provides a kind of processing method, described method by toasting tobacco through fire provide the component at least partially of special sense characteristic (that is, cigarette fragrance and fragrance) with desired by not promoting on significance degree in fire toasts tobacco with the Component seperation at least partially of special sense quality.In other words, the invention provides a kind of separation method, described method choice ground extracts to toast tobacco component through fire desired by sensation viewpoint, but remaining from sensation viewpoint do not need or those components undesirable at least partially.

When method of the present invention is applied to toast tobacco material through fire time, extract can be formed in certain embodiments, it is characterized in that with the sense quality of the relevant hope that toasts tobacco through fire (such as, cigarette fragrance and fragrance), but there is the chemical characteristic of change, be included in some polycyclic aromatic hydrocarbon, such as benzo [a] pyrene (that is, BaP or B [a] minimizing p) common in fire toasts tobacco.Give the structure of BaP below.

Benzo [a] pyrene

The discussion of BaP and other polycyclic aromatic hydrocarbon, can be see: Gelboin, Physiological Reviews 60 (4) (1980) 1107-1166; Phillips, Mutation Research 443 (1999) 139-147; Rodgman and Perfetti, Contributions to Tobacco Research 22 (1) (2006) 13-69; Rodgman and Cook, Contributions to Tobacco Research 23 (6) (2009) 384-410; With A.Rodgman and T.A.Perfetti, The Chemical Components of Tobacco and Tobacco Smoke, CRC Press, Taylor and Francis Group, Boca Raton, USA, (2009), they are incorporated to herein all by reference.

Make it possible to produce such smoking product and smokeless tobacco composition through the fire extract that toasts tobacco containing the polycyclic aromatic hydrocarbon level reduced: it shows toasting tobacco sense quality through fire of hope, but has the content of the compound (such as BaP) irrelevant with the sense quality of described hope of reduction.It should be pointed out that as understood in the art, feel grade form by end user, the sense quality of composition can be evaluated.

Although BaP content can change based on the specific tobacco plant adopted and concrete fiery curing process, the typical BaP scope toasted tobacco through fire is about 150 to about 8,000 hundred million parts (ppb).In certain embodiments of the invention, can be formed there is toasting tobacco extract through fire of significantly lower BaP level (be such as less than about 10ppb, be less than about 5ppb or be even less than about 1ppb).In other words, the amount that the BaP occurred in leaching process of the present invention reduces can be characterized by, and the BaP content in original undrawn tobacco-containing material have dropped at least about 90 % by weight, more commonly at least about 95% or at least about 99%.Unknown so far, can be formed and such to toast tobacco extract through fire: it retains the special sense component of such tobacco, but it shows the content of some chemical compound of not too wishing (such as BaP) of reduction.In an embodiment of method of the present invention, through described leaching process the tobacco-containing material through baking (such as, toast tobacco through fire) there is following BaP concentration: at least about 100ppb, more frequent at least about 150ppb, or even at least about 200ppb or at least about 300ppb.After described leaching process, the extract of described separation shows lower BaP concentration far away, is such as no more than about 10ppb or is no more than about 5ppb or is no more than the concentration of about 1ppb.

For determining that the multiple method of BaP content is known in the art.Usually, described method comprises: from tobacco-containing material, extract BaP with the solvent (such as hexane, cyclohexane or carrene) of methyl alcohol or relative non-polarity.Then filter described extract, and use and there is the high performance liquid chromatography (HPLC) of fluoroscopic examination or gas chromatography-mass spectrography (GC-MS) technology is analyzed.The publication of the extraction and detection that relate to the BaP in tobacco or tobacco product comprises: Rodgman and Perfetti, Contributions to Tobacco Research 22 (1) (2006) 13-69; Risner, Beitr.Tabakforsch.Int.15 (1) (1991) 11-17; " Determination of Benzo [a] Pyrene in Whole Tobacco; " Health Canada (1999) (is disclosed on Health Canada website, www.hc-sc.gc.ca), the people such as Ayg ü n, International Journal of Food Sciences and Nutrition 56 (8) (2005) 581-585; With the people such as McNeill, Tob.Control 15 (2006) 64-67, they are incorporated to herein all by reference.

Toasting tobacco through fire of using in the method for the invention can be included in those tobacco-containing materials conventional in fiery baking, such as Narrow Leaf Madole, Improved Madole, Tom Rosson Madole, Newton's VH Madole, Little Crittenden, Green Wood, Little Wood, Small Stalk Black Mammoth, DT 508, DT 518, DT 592, KY 171, DF 911, DF 485, TN D94, TN D950, VA 309 and VA 359.But, any tobacco-containing material can be used and do not depart from the present invention, comprise those tobaccos being commonly referred to as following title: the tobacco of flue baking or Virginia tobacco are (such as, K326), burley, the tobacco of drying (such as, India Kurnool and Oriental tobacco, comprise Katerini, Prelip, Komotini, Xanthi and Yambol tobacco), Maryland tobacco, dark tobacco, dark air-dry tobacco (such as, Passanda, Cubano, Jatin and Bezuki tobacco), the air-dry tobacco of light breeze (such as, North Wisconsin and Galpao tobacco), the tobacco that India is air-dry, Red Russian tobacco and Rustica tobacco and other rare or special tobacco various.At Tobacco Production, Chemistry and Technology, in the people such as Davis (volume) (1999) (it is incorporated to herein by reference), set forth the description that dissimilar tobacco, cultivation practices and results are put into practice.From the various representational vegetation type of Nicotiana kind see Goodspeed, The Genus Nicotiana, (Chonica Botanica) (1954); The U.S. Patent number 4,660,577 of the people such as Sensabaugh, Jr.; The U.S. Patent number 5,387,416 of the people such as White, and the U.S. Patent number 7,025,066 of the people such as Lawson; The U.S. Patent Application Publication No. 2006/0037623 of Lawrence, Jr., and the U.S. Patent Application Publication No. 2008/0245377 of the people such as Marshall; They every section be incorporated to herein by reference.In one embodiment, in leaching process of the present invention, use such tobacco bred: it carrys out baking by the baking technique except baking except fire usually, such as flue baking or air-dry.If necessary, the roasting process of the fire traditional baking technique substituted for this material can be optionally used to carry out the such tobacco-containing material of baking.

The specific Nicotiana kind material used in the present invention also can change.Interested is especially safflower tobacco (N.tabacum), makhorka (N.rustica), Henbane (N.alata), N.arentsii, N.excelsior, Fu Erjiteshi tobacco (N.forgetiana), powder blue smoke grass (N.glauca), sticky tobacco (N.glutinosa), brother Xi Shi tobacco (N.gossei), slips card Michaelis tobacco (N.kawakamii), Nai Teshi tobacco (N.knightiana), Lang Shi tobacco (N.langsdorffi), ear tobacco (N.otophora), Sai Teshi tobacco (N.setchelli), woods tobacco (N.sylvestris), velvet tobacco (N.tomentosa), fine hair shape tobacco (N.tomentosiformis), ripple leaf tobacco (N.undulata) and Henbane (N.x sanderae).Also interested is African tobacco (N.africana), embrace stem tobacco (N.amplexicaulis), Bei Namoteshi tobacco (N.benavidesii), rich tobacco (N.bonariensis) inside, Di Bonashi tobacco (N.debneyi), long luxuriant tobacco (N.longiflora), beach tobacco (N.maritina), especially big pipe tobacco (N.megalosiphon), west tobacco (N.occidentalis), circular cone tobacco (N.paniculata), blue arabian jasmine leaf tobacco (N.plumbaginifolia), Lei Mengdeshi tobacco (N.raimondii), lotus sits leaf tobacco (N.rosulata), makhorka (N.rustica), intend like tobacco (N.simulans), stoke Tong Shi tobacco (N.stocktonii), fragrant and sweet tobacco (N.suaveolens), Nicotiana tabacum (N.tabacum), bright (N.umbratica), quiver a mao tobacco (N.velutina) and parsley tobacco (N.wigandioides).Other plant from Nicotiana kind comprises: acaulescence tobacco (N.acaulis), acuminate tobacco (N.acuminata), gradually narrow leaf tobacco (N.attenuata), Ben Saimushi tobacco (N.benthamiana), hole uncured tobacco (N.cavicola), Ke Lifulanshi tobacco (N.clevelandii), lobus cardiacus tobacco (N.cordifolia), umbrella bed tobacco (N.corymbosa), cigarette grass (N.fragrans), Gu Tesi Bi Shi tobacco (N.goodspeedii), narrow leaf tobacco (N.linearis), Mo Xishi tobacco (N.miersii), naked stem tobacco (N.nudicaulis), Ou Butesi tobacco (N.obtusifolia), thrips cigarette Hersperis subspecies (N.occidentalis subsp.Hersperis), few Henbane (N.pauciflora), petunia shape tobacco (N.petunioides), Kua Deruiwushi tobacco (N.quadrivalvis), residual wave tobacco (N.repanda), roundleaf tobacco (N.rotundifolia), eggplant tobacco (N.solanifolia) and Si Peigeci tobacco (N.spegazzinii).Use genetic modification or crossbreeding technology, Nicotiana kind can be derived (such as, genetically engineered or crossbreeding can be carried out, to increase or to reduce the generation of some component or otherwise to change some proterties or feature) to tobacco plant.See, such as, the type of the genetic modification of the plant of setting forth in following document: the U.S. Patent number 5,539,093 of the people such as Fitzmaurice; The U.S. Patent number 5,668,295 of the people such as Wahab; The U.S. Patent number 5,705,624 of the people such as Fitzmaurice; The U.S. Patent number 5,844,119 of Weigl; The U.S. Patent number 6,730,832 of the people such as Dominguez; The U.S. Patent number 7,173,170 of the people such as Liu; The U.S. Patent number 7,208,659 of the people such as Colliver, and the U.S. Patent number 7,230,160 of the people such as Benning; The U.S. Patent Application Publication No. 2006/0236434 of the people such as Conkling; With the PCT WO 2008/103935 of the people such as Nielsen.

Can using (namely with prematurity form at least partially of Nicotiana plant, can before reaching and it has been generally acknowledged that ripe or overdue stage, such as, when tobacco plant be in sprout some time, start to form leaf time, start to bloom time etc., results plant or plant are at least partially).Can the using with mature form at least partially of described plant (that is, when plant (or plant part) reach think traditionally at ripe, overdone or overdue some time, described plant or plant can be gathered in the crops at least partially).Such as, tobacco results technology like this, by using farmer to commonly use, spices tobacco plant can be gathered in the crops, burley plant can be gathered in the crops, maybe can gather in the crops Virginia tobacco leaf, or gather in the crops (prime) according to genius loci (stalk position).Aging condition can also be carried out to the tobacco-containing material used in the present invention.

In certain embodiments, described plant can use (such as, can use tobacco when not carrying out any cooking process) with blue or green form.Such as, freezing, irradiation, yellow, drying, the cooking (such as, roasting, fried or boil) can be carried out to the tobacco of blue or green form, or otherwise carry out storing or processing, for later use.Aging condition can also be carried out to such tobacco.

According to the present invention, the tobacco-containing material of any type that results are pointed out above, and carry out baking technique, such as fiery curing process.Then some polar aprotic solvent is used, such as water, formic acid, acetic acid, dilute aqueous solution are (such as, comprise and be greater than the water of 70 % by weight and the solution of in a small amount alcohol or other cosolvent) or their mixture, carry out leaching process to what obtain through baking tobacco.Described solvent usually have be at least about 6 in room temperature, more frequent at least about 30 and the most frequent at least about 50 dielectric constant.

The solvent with aqueous nature is useful especially, such as deionized water, distilled water or running water.Such solvent forms primarily of water, is normally greater than the water of 90 % by weight, and can be substantially pure water in some cases.Described Extraction solvent can be cosolvent mixture, the mixture of such as water and the in a small amount solvent that one or more can be miscible with one another.An example of such cosolvent mixture is, the solvent be made up of the water of about 95 weight portions and the ethanol of about 5 weight portions.Described Extraction solvent also can comprise such water: it contains materials such as being such as dissolved in pH adjusting agent wherein (that is, acid or alkali) or pH buffer.

Described leaching process comprises: make described tobacco-containing material and the described solvent time period that intimate contact is suitable at a suitable temperature.Extracting temperature can change, but typical temperature range be about room temperature to about 110 DEG C, more often about 30 DEG C to about 90 DEG C.In certain embodiments, the temperature of described extraction step can be characterized by least about 20 DEG C, at least about 30 DEG C, at least about 50 DEG C or at least about 60 DEG C.May it is appropriate that use relatively low temperature for described leaching process, to prevent or to reduce the volatilization of compound of good to eat or aromatics of the major target as leaching process.

The time period of described extraction step can change, but normally about 10 minutes to about 24 hours, more often about 1 is little of about 12 hours.Think that the described time period is not crucial especially for the present invention, although very short extraction time section may can not cause the major part of tobacco-containing material can the extraction of extraction components.

The amount of the solvent used in described leaching process can change, but is usually enough to make tobacco-containing material form the form of slurry.In other words, the advantage component of solvent normally tobacco/solvent mixture, and often greatly excessively exist relative to tobacco ingredient.The weight ratio of solvent and tobacco-containing material, usually in the scope of about 2:1 to about 20:1 (such as, about 4:1 to about 12:1), although can use other ratio (particularly even larger ratio), and does not depart from the present invention.In certain embodiments, water more in a small amount or the use of other solvent are favourable, because if before the use must concentrated extract, will need less drying.The over-drying meeting of extract causes the loss of the component of the volatile good to eat or aromatics of some of described extract, and this can cause the loss of some special sense characteristic of described extract potentially.Therefore, using in leaching process and be less than about 5:1 or be less than the solvent of about 4:1 and the weight ratio of tobacco-containing material, reducing or eliminating being useful technology that is dry or the otherwise demand of the concentrated extract obtained.In such a embodiment, expect that described extract can show relatively high viscosity, and some tobacco product can be applied to without adding further building site.

Mode solvent and tobacco-containing material being mixed mutually carry out extracting can change.Can in pyramid type blender, mixing drum, band shape blender etc., solvent be contacted with tobacco-containing material, combine or mix.During extraction step, described mixture can be stirred, or carry out grinding operation.After extraction, use any means known in the art, such as filtration or centrifugal, from liquid extraction product, remove remaining slurry.In leaching process, described tobacco-containing material is fragment or particulate form normally, such as has the tobacco particle of the granularity within the scope of about 0.5mm to about 25mm.The container of smoking mixture material and solvent has exhaust outlet usually wherein, is extracted in normal pressure and carries out described in making, or if necessary, can use pressurized container.After leaching process, by from solvent and be dissolved or dispersed in solvent soluble wherein or isolate the insoluble pulp material of solvent in dispersible tobacco ingredient, tobacco extract is provided.

For obtaining the equipment of tobacco extract, type of solvent and technology, be included in the equipment, solvent and the technology that may be used in some cases in method of the present invention or be for carrying out suitably improvement in method of the present invention, see: the U.S. Patent number 4,144,895 of Fiore; The U.S. Patent number 4,150,677 of the people such as Osborne, Jr.; The U.S. Patent number 4,267,847 of Reid; The U.S. Patent number 4,289,147 of the people such as Wildman; The U.S. Patent number 4,351,346 of the people such as Brummer; The U.S. Patent number 4,359,059 of the people such as Brummer; The U.S. Patent number 4,506,682 of Muller; The U.S. Patent number 4,589,428 of Keritsis; The U.S. Patent number 4,605,016 of the people such as Soga; The U.S. Patent number 4,716,911 of the people such as Poulose; The U.S. Patent number 4,727,889 of the people such as Niven, Jr.; The U.S. Patent number 4,887,618 of the people such as Bernasek; The U.S. Patent number 4,941,484 of the people such as Clapp; The U.S. Patent number 4,967,771 of the people such as Fagg; The U.S. Patent number 4,986,286 of the people such as Roberts; The U.S. Patent number 5,005,593 of the people such as Fagg; The U.S. Patent number 5,018,540 of the people such as Grubbs; The U.S. Patent number 5,060,669 of the people such as White; The U.S. Patent number 5,065,775 of Fagg; The U.S. Patent number 5,074,319 of the people such as White; The U.S. Patent number 5,099,862 of the people such as White; The U.S. Patent number 5,121,757 of the people such as White; The U.S. Patent number 5,131,414 of Fagg; The U.S. Patent number 5,131,415 of the people such as Munoz; The U.S. Patent number 5,148,819 of Fagg; The U.S. Patent number 5,197,494 of Kramer; The U.S. Patent number 5,230,354 of the people such as Smith; The U.S. Patent number 5,234,008 of Fagg; The U.S. Patent number 5,243,999 of Smith; The U.S. Patent number 5,301,694 of the people such as Raymond; The U.S. Patent number 5,318,050 of the people such as Gonzalez-Parra; The U.S. Patent number 5,343,879 of Teague; The U.S. Patent number 5,360,022 of Newton; The U.S. Patent number 5,435,325 of the people such as Clapp; The U.S. Patent number 5,445,169 of the people such as Brinkley; The U.S. Patent number 6,131,584 of Lauterbach; The U.S. Patent number 6,298,859 of the people such as Kierulff; The U.S. Patent number 6,772,767 of the people such as Mua; With the U.S. Patent number 7,337,782 of Thompson, they are incorporated to herein all by reference.

After slurry separating extractive, if necessary, extract and remaining slurry can be processed further.Such as, can by removing solvent at least partially, with can concentrate the dissolving of tobacco-containing material or the mode of component of dispersion process extract.Can use various solvent removal process, such as heat treatment is with evaporating solvent (such as, with evaporimeter and condenser arrangement), reverse osmosis membrane processing, spraying dry or freeze drying.When aqueous extract, concentration step only needs temperature extract being heated above water boiling point in ventilated container.Also can carry out other processing method of the chemical composition for changing extract to extract, such as with the ultrafiltration of acid or alkali reaction, removing high molecular weight component, remove the process etc. of other component (the specific nitrosamine of such as tobacco (TSNA)) of extract.

In one particular embodiment, processing is substantially free of the extract of BaP, to reduce the concentration of the TSNA in described extract.Exemplary TSNA compound comprises: N-nitrosonornicotine (NNN), 4-methyl-N-nitrosamino--1-(3-pyridine radicals)-1-butanone (NNK), N-nitrosoanatabine (NAT), 4-methyl-N-nitrosamino--1-(3-pyridine radicals)-n-butyl alcohol (NNAL) and N-nitroso alangine (NAB).Method for reducing TSNA level can change.In one approach, use preparation HPLC technology, wherein make described extract through HPLC column, and be discarded in the part of known retention time from the extract of post wash-out of TSNA compound simply.In another approach, make described extract through molecularly imprinted polymer (MIP) material, described material has the functional group of optionally adsorbing TSNA compound.The specific MIP material of exemplary TSNA-comprises: by Sigma-Aldrich Company in brand name the polymer absorbant provided under SPE, and the Affinilute that can obtain from Biotage AB ^tMmIP material.Use multiple technologies, such as with described adsorbent packed column, and make described extract through this post, polymeric adsorbant can be made to contact with described extract, optionally to adsorb TSNA compound.In certain embodiments, the TSNA level of described extract can be made to be reduced to and to be less than about 400ppb from being greater than 1,000ppb or being even greater than 2,000ppb or to be less than about 300ppb or to be less than about 200ppb.In some cases, TSNA level can be made to be reduced to be less than about 100ppb or be less than about 50ppb.

In one embodiment, the remaining tobacco pulp that produces in described leaching process can be processed to reduce benzo [a] pyrene concentration, thus recombinate the slurry of the reconstruct tobacco-containing material to form benzo [a] the pyrene concentration showing reduction for the preparation of with described extract.Such as, use supercritical carbon dioxide or other suitable solvent (such as, solvent such as hexane, cyclohexane or the carrene of relative non-polarity), second extraction process can be carried out to described slurry, benzo [a] pyrene is dissolved in a solvent to promote the removing from described slurry.To may be used in the present invention or for for carry out in the present invention the carbon dioxide draw technique suitably improved see: such as, the U.S. Patent number 4,153,063 of the people such as Roselius; The U.S. Patent number 4,506,682 of Muller; The U.S. Patent number 4,714,617 of Gahrs; The U.S. Patent number 4,727,889 of the people such as Niven, Jr.; The U.S. Patent number 5,018,540 of the people such as Grubbs; With the U.S. Patent number 5,435,325 of the people such as Clapp, they are incorporated to herein all by reference.

In certain embodiments, the supercritical CO as further described in this article is carried out to described tobacco pulp ₂extract.Usually, supercritical fluid extraction is by supercritical CO ₂add in tobacco pulp, to promote that some component (such as, B [a] p and TSNA) is from the removing of tobacco pulp.Described extraction can use and can make tobacco and supercritical CO ₂the equipment of any type of contact carries out.Such as, in some specific embodiments, can use and such as can derive from Jasco, the supercritical fluid extraction system of Inc. (Easton, MD).In certain embodiments, pure supercritical CO ₂it is Extraction medium; But, in certain embodiments, may use except supercritical CO ₂also comprise the Extraction medium of one or more components in addition.Leaching process can utilize downstream reflux medium (such as, methyl alcohol), to trap the compound extracting (that is, removing) from tobacco-containing material.

Supercritical CO can be changed ₂the various parameters of leaching process.In certain embodiments, the one or more efficiency that can change leaching process in these parameters are changed.Such as, pressure, temperature, CO can be changed ₂flow velocity and total extraction time.Such as, in certain embodiments, the pressure of about 10MPa or larger is used, and the pressure of more preferably from about 20MPa or larger.Such as, in certain embodiments, use about 5MPa to the pressure of about between 40MPa (such as, about 10MPa is to about between 40MPa, or about 10MPa is to about between 30MPa).In certain embodiments, use about 40 DEG C or larger temperature, and more preferably, use about 60 DEG C or larger temperature.Such as, in certain embodiments, the temperature of (such as, between about 40 DEG C to about 60 DEG C) between about 30 DEG C to about 70 DEG C is used.In certain embodiments, use the flow velocity of about 5mL/min or larger, and more preferably, use the flow velocity of about 10mL/min or larger.Such as, in certain embodiments, use about 4mL/min to the flow velocity of about between 15mL/min (such as, about 5mL/min is to about between 10mL/min).

In certain embodiments, total extraction time is about 10 minutes or more, about 15 minutes or more or about 30 minutes or more.Usually, total extraction time of about 15 minutes or more can cause the good removing of B [a] p and TSNA (such as, B [a] p and TSNA be greater than about 50% removing).In certain embodiments, total extraction time of about 30 minutes or more can provide even larger B [a] p and TSNA to remove.It should be pointed out that in certain embodiments, higher or lower temperature, higher or lower flow velocity and/or higher or lower total extraction time can be utilized to provide good result (that is, the remarkable decline of the concentration of B [a] p and/or TSNA).

Wherein supercritical CO is passed through at some ₂extract the tobacco pulp that carries out processing to have carried out in the past in the embodiment that water extraction gets, the treated slurry obtained can be characterized by " two extraction " tobacco pulp.Thus the slurry of two extraction comprises such slurry: wherein got by water extraction and eliminated aqueous components, and through supercritical CO ₂extraction eliminates other component.

Supercritical CO ₂leaching process can cause being present in the minimizing of the amount of B [a] p in tobacco-containing material and/or the amount of TSNA usually.In certain embodiments, with not through supercritical CO ₂the tobacco of extraction process is compared, described supercritical CO ₂extraction can provide B [a] p of about 5% or more, about 10% or more, about 20% or more, about 30% or more, about 40% or more, about 50% or more, about 60% or more, about 70% or more or about 80% or more to reduce.Usually, not through supercritical CO ₂the tobacco of extraction process can have and is greater than about 50ng/g, is greater than about 100ng/g, is greater than about 150ng/g or is greater than B [a] the p level of about 200ng/g.In certain embodiments, can by through supercritical CO ₂the tobacco pulp of extraction process is characterized by have and is less than about 150ng/g, is less than about 100ng/g, is less than about 80ng/g or is less than about 50ng/g.In certain embodiments, with not through supercritical CO ₂the tobacco of extraction process is compared, described supercritical CO ₂extraction can provide the TSNA of about 5% or more, about 10% or more, about 20% or more, about 30% or more, about 40% or more, about 50% or more, about 60% or more, about 70% or more or about 80% or more to reduce.Usually, not through supercritical CO ₂the tobacco of extraction process can have and is greater than about 2,500ng/g, is greater than about 5,000ng/g, is greater than about 7,500ng/g, or is greater than the TSNA level of about 10,000ng/g.In certain embodiments, can by through supercritical CO ₂the tobacco pulp of extraction process is characterized by have and is less than about 5,000ng/g, is less than about 7,500ng/g, is less than about 5,000ng/g, is less than about 2,000ng/g or be less than about 1,000ng/g.

After this, by by the extract add-back from preliminary extraction process through pretreated slurry (such as, by slurry that supercritical carbon dioxide extraction process is crossed), the tobacco-containing material of reconstruct can be formed.For providing exemplary mode and the method for reconstruct tobacco sheet, comprise casting technique and paper technology, see: the U.S. Patent number 4,674,519 of the people such as Keritsis; The U.S. Patent number 4,941,484 of the people such as Clapp; The U.S. Patent number 4,987,906 of the people such as Young; The U.S. Patent number 4,972,854 of the people such as Kiernan; The U.S. Patent number 5,099,864 of the people such as Young; The U.S. Patent number 5,143,097 of the people such as Sohn; The U.S. Patent number 5,159,942 of the people such as Brinkley; The U.S. Patent number 5,322,076 of the people such as Brinkley; The U.S. Patent number 5,339,838 of the people such as Young; The U.S. Patent number 5,377,698 of the people such as Litzinger; The U.S. Patent number 5,501,237 of Young; With the U.S. Patent number 6,216,707 of Kumar; Each section in them is incorporated to herein by reference.Also extract and reconstruct tobacco process see the tobacco of setting forth in the U.S. Patent number 5,360,022 (they are incorporated to herein by reference) of the people such as the U.S. Patent number 5,065,775 of Fagg and Newton.

Can also carry out preprocessing process to the tobacco-containing material carrying out leaching process, described preprocessing process can change the sensation of described material, chemistry or physical property.Such as, may wish that pre-treat tobacco material can produce the tobacco ingredient of negative cacesthesia feature with removing, make can not extract those components in the method for the invention.The exemplary preprocessing process of tobacco-containing material comprises fermentation, bleaching etc.

In certain embodiments of the invention, advantageously, pretreatment toasts tobacco to change sense quality through fire in a specific way, and described mode can be characterized by the fragrance or fragrance that produce milder.Can the generation fragrance of milder or a kind of illustrative methods of fragrance be fermentation in some tobacco-containing material (such as toasting tobacco through fire).During the fermentation, bacterium humidity, temperature control with control pH environment in interact with tobacco-containing material, to change the chemical characteristic of tobacco-containing material.The tobacco-containing material be by fermentation obtained commercially may be used in leaching process of the present invention, such as the snuff tobacco compositions of the humidity of GRIZZLY or KODIAK smokeless tobacco sale.Tobacco fermentation technique see, such as, the people such as Giacomo, Appl.Environ.Microbiol.73 (3) (2007) 825-837; The U.S. Patent number 5,372,149 of the people such as Roth; With Tobacco Production, Chemistry and Technology, the people such as Davis (volume) (1999)), they are incorporated to herein all by reference.

Tobacco extract can be used as the good to eat tobacco compositions that can mix in multiple tobacco product.Particularly, of the present inventionly different tobacco products can be given by the special sense characteristic toasted tobacco through fire through the fire extract that toasts tobacco, and that do not introduce significant quantity with undrawn or complete some chemical compound toasting tobacco relevant through fire, such as BaP.Tobacco extract (such as, water-based tobacco extract) can be used in a variety of forms.Such as, the form separate tobacco extract of solvent can be substantially free of, such as can be used as and use the result of the procedure of processing of spraying dry or freezing dry process or other similar type and obtain.Alternatively, the water-based tobacco extract of liquid form can be adopted, and like this, the content of the tobacco DDGS in liquid flux can be controlled as follows: by selecting the amount for the solvent extracted, by removing solvent concentration liquid tobacco extract, add solvent with diluent liquid tobacco extract, or similar method.

The tobacco product adding extract of the present invention wherein can change, and comprises any product being configured to maybe tobacco or its some component to be delivered to the user of product.Exemplary tobacco product comprises smoking product (such as, cigarette), smokeless tobacco product and the aerocolloidal device of generation, and described device contains in use incombustible tobacco-containing material or other vegetable material.

Usually, extract of the present invention will comprise to mixing in tobacco product, use tobacco-containing material or non-tobacco vegetable material as the carrier of extract, such as by described extract being adsorbed in tobacco or other vegetable material, or otherwise make described extract be combined with carrier material, such as by spray-dired extract particles being attached on carrier material.The type that can be used as the tobacco of the carrier of extract of the present invention can change, and any tobacco type discussed can be comprised herein, comprise the various tobacco-containing material through baking (such as, that flue toasts or dry tobacco) or its part (such as, tobacco sheet or tobacco stem).In one embodiment, be through the tobacco-containing material of fermentation to its tobacco applying described extract, and before sweat, in process or after-applied described extract.The tobacco-containing material applying described extract to it is characterized as being usually, has relatively low BaP level, the tobacco-containing material of such as many that dry or flue bakings or through pretreatment to reduce the tobacco-containing material of BaP level.The physical configuration adding the tobacco-containing material of described extract to it also can change, and can comprise the tobacco-containing material of following form: fragment or particulate form, or sheet form (such as, reconstruct tobacco sheet), or intact leaves form.Tobacco-containing material can change with the dry weight ratio of extract of the present invention, but normally about 4:1 is to about 1:4, about 2:1 to about 1:2, is often about 1.5:1 to about 1:1.5.

In one embodiment, extract of the present invention is used as good to eat tobacco compositions in the manufacture of smoking product.Such as, extract prepared in accordance with the present invention can mix mutually with sheathing material, and is applied to tobacco as jacket ingredients and (such as, is used in the U.S. Patent number 4 of Shelar, 819, the Method type of setting forth in 668, it is incorporated to herein by reference), mix in smoking product as top flavoring ingredients, or to mix in the tobacco-containing material of reconstruct (such as, be used in the tobacco restructuring processes type usually set forth in following U.S. Patent number: 5,143,097 of Sohn; The people's such as Brinkley 5,159,942; 5,598,868 of Jakob; 5,715,844 of Young; 5,724,998 of Gellatly; With 6,216,706 of Kumar, they are incorporated to herein by reference).Further, in cigarette manufacturing processes, extract of the present invention can mix (such as, in filter tip bung, forming paper or tipping paper) in cigarette filter, or mixes in cigarette wrapper, preferably on an internal surface.

Be the smoking product 10 of cigarette form shown in Fig. 1, it has some representational component that can contain the smoking product of extract of the present invention.Cigarette 10 comprises and is comprised in the usual cylindrical bar 12 that in circumscribing wrapping material 16 or a volume can aspirate packing material (such as about 0.3 can aspirate packing material to about 1.0g, such as tobacco-containing material).Bar 12 is commonly called " tobacco rod ".The end of tobacco rod 12 is open, can aspirate packing material to expose.Cigarette 10 is shown as has the optional band 22 of of being attached on described packaging material 16 (such as, print coating, comprise film forming agent, as starch, ethyl cellulose or sodium alginate), this band surrounds cigarette carton on the direction of the longitudinal axis crosscut with cigarette.(that is, in the face of can packing material be aspirated) on the inner surface of packaging material can be printed on 22, or less preferably, be printed on the outer surface of described packaging material.

Tobacco rod 12 one end lights end 18, and at mouth end 20, place is provided with filter element 26.Described filter element 26 is positioned at the adjacent one end of tobacco rod 12, makes described filter element and tobacco rod be axially-aligned with end-to-end relation, preferably adjacent one another are.Filter element 26 can have common cylinder form, and its diameter can be substantially equal to the diameter of tobacco rod.The two ends of filter element 26 allow air and smog to pass through wherein.

Adopt optional air dilution means, as a series of hole 30 (each hole penetrates tipping material 44 and forming paper 28), can provide ventilation or Dilution air smoking product.Adopt various technology known to persons of ordinary skill in the art, as laser drilling, optional hole 30 can be made.Alternatively, so-called off-line Dilution air technology (such as, by using the tipping paper of porous, shaped paper and pre-punching) can be adopted.

Extract of the present invention also can mix and produce in aerocolloidal device, and described device contains the tobacco-containing material (or its some part or component) of in use not wishing to burn.Describe generation fragrance gas, as seen the exemplary reference document of the smoking product of the type of aerosol or fragrance gas and visible aerocolloidal mixture to comprise: the U.S. Patent number 3,258,015 of the people such as Ellis; The U.S. Patent number 3,356,094 of the people such as Ellis; The U.S. Patent number 3,516,417 of Moses; The U.S. Patent number 4,347,855 of the people such as Lanzellotti; The U.S. Patent number 4,340,072 of the people such as Bolt; The U.S. Patent number 4,391,285 of the people such as Burnett; The U.S. Patent number 4,917,121 of the people such as Riehl; The U.S. Patent number 4,924,886 of Litzinger; With the U.S. Patent number 5,060,676 of the people such as Hearn, they are incorporated to herein all by reference.Many employing ignitable fuel sources in the smoking product of these types, the latter is burned to provide aerosol and/or heat air colloidal sol to form material.See, such as, the U.S. Patent number 4,756,318 of the people such as Clearman; The U.S. Patent number 4,714,082 of the people such as Banerjee; The U.S. Patent number 4,771,795 of the people such as White; The U.S. Patent number 4,793,365 of the people such as Sensabaugh; The U.S. Patent number 4,917,128 of the people such as Clearman; The U.S. Patent number 4,961,438 of Korte; The U.S. Patent number 4,966,171 of the people such as Serrano; The U.S. Patent number 4,969,476 of the people such as Bale; The U.S. Patent number 4,991,606 of the people such as Serrano; The U.S. Patent number 5,020,548 of the people such as Farrier; The U.S. Patent number 5,033,483 of the people such as Clearman; The U.S. Patent number 5,040,551 of the people such as Schlatter; The U.S. Patent number 5,050,621 of the people such as Creighton; The U.S. Patent number 5,065,776 of Lawson; The U.S. Patent number 5,076,296 of the people such as Nystrom; The U.S. Patent number 5,076,297 of the people such as Farrier; The U.S. Patent number 5,099,861 of the people such as Clearman; The U.S. Patent number 5,105,835 of the people such as Drewett; The U.S. Patent number 5,105,837 of the people such as Barnes; The U.S. Patent number 5,115,820 of the people such as Hauser; The U.S. Patent number 5,148,821 of the people such as Best; The U.S. Patent number 5,159,940 of the people such as Hayward; The U.S. Patent number 5,178,167 of the people such as Riggs; The U.S. Patent number 5,183,062 of the people such as Clearman; The U.S. Patent number 5,211,684 of the people such as Shannon; The U.S. Patent number 5,240,014 of the people such as Deevi; The U.S. Patent number 5,240,016 of the people such as Nichols; The U.S. Patent number 5,345,955 of the people such as Clearman; The U.S. Patent number 5,551,451 of the people such as Riggs; The U.S. Patent number 5,595,577 of the people such as Bensalem; The U.S. Patent number 5,819,751 of the people such as Barnes; The U.S. Patent number 6,089,857 of the people such as Matsuura; The U.S. Patent number 6,095,152 of the people such as Beven; The U.S. Patent number 6,578,584 of Beven; With the U.S. Patent number 6,730,832 of Dominguez; They are incorporated to herein by reference.In addition, the cigarette of some type of carbonaceous fuel element is adopted to be put on market to business under brand name " Premier " and " Eclipse " by R.J.Reynolds Tobacco Company.See, such as, those cigarettes types described in following document: Chemical and Biological Studies on New Cigarette Prototypes that Heat Instead of Burn Tobacco, R.J.Reynolds Tobacco Company Monograph (1988) and Inhalation Toxicology, 12:5,1-58 page (2000).The aerocolloidal device of generation of other type see: the U.S. Patent number 7,726,320 of the people such as Robinson, and the U.S. Patent Application Publication No. 2006/0196518 and 2007/0267031 of Hon, they are incorporated to herein all by reference.

Extract of the present invention can mix in smokeless tobacco product, the moist snuff (such as, snus) that described smokeless tobacco product is such as loose, loose dry snuff, chewing tobacco, graininess tobacco sheet (such as, has ball, sheet, ball, coin, pearl, the shape of oranges and tangerines (obloids) or beans), extruding or the tobacco rods formed, sheet, rod, cylinder or rod, the milled powder of fine crushing, fine crushing or Powdered and the agglomerate of component of grinding, flake sheet, the tobacco sheet of molding processing, chewing gum tablet containing tobacco, belt type film is rolled up, film that is soluble in water or that dispersible in water or bar (such as, the U.S. Patent Application Publication No. 2006/0198873 of the people such as Chan), or to have shell (can be such as, transparent in nature, colourless, translucent or highly colored softness or hard shell) and the capsule shape material of interior zone containing tobacco or tobacco spice (such as, the Newtonian fluid of the tobacco of some kinds form or thixotropic fluid).Dissimilar smokeless tobacco product is see the U.S. Patent number 1,376,586 of Schwartz; The U.S. Patent number 3,696,917 of Levi; The U.S. Patent number 4,513,756 of the people such as Pittman; The people such as the U.S. Patent number 4,528,993, Jr. of Sensabaugh; The U.S. Patent number 4,624,269 of the people such as Story; The U.S. Patent number 4,987,907 of Townsend; The U.S. Patent number 5,092,352 of the people such as Sprinkle, III; With the U.S. Patent number 5,387,416 of the people such as White; The U.S. Patent Application Publication No. 2008/0196730 of the people such as the U.S. Patent Application Publication No. 2005/0244521 of the people such as Strickland and Engstrom; The PCT WO 04/095959 of the people such as Arnarp; The PCT WO 05/063060 of the people such as Atchley; The PCT WO 05/016036 of Bjorkholm; With the PCT WO 05/041699 of the people such as Quinter, each section in them is incorporated to herein by reference.Also see the type of, the smokeless tobacco preparation of setting forth in following document, composition and processing method: the U.S. Patent number 7,032,601 of the people such as the U.S. Patent number 6,953,040 of the people such as Atchley and Atchley; The U.S. Patent Application Publication No. 2002/0162562 of Williams; The U.S. Patent Application Publication No. 2002/0162563 of Williams; The U.S. Patent Application Publication No. 2003/0070687 of the people such as Atchley; The U.S. Patent Application Publication No. 2004/0020503 of Williams; The U.S. Patent Application Publication No. 2005/0178398 of the people such as Breslin; The U.S. Patent Application Publication No. 2006/0191548 of the people such as Strickland; The U.S. Patent Application Publication No. 2007/0062549 of the people such as Holton, Jr.; The U.S. Patent Application Publication No. 2007/0186941 of the people such as Holton, Jr.; The U.S. Patent Application Publication No. 2007/0186942 of the people such as Strickland; The U.S. Patent Application Publication No. 2008/0029110 of the people such as Dube; The U.S. Patent Application Publication No. 2008/0029116 of the people such as Robinson; The U.S. Patent Application Publication No. 2008/0029117 of the people such as Mua; The U.S. Patent Application Publication No. 2008/0173317 of the people such as Robinson; The U.S. Patent Application Publication No. 2008/0209586 of the people such as Neilsen; The U.S. Patent Application Publication No. 2010/0018541 of the people such as Gerardi; The U.S. Patent Application Publication No. 2010/0018540 of the people such as Doolittle; With the U.S. Patent Application Publication No. 2010/0116281 of the people such as Marshall, each section in them is incorporated to herein by reference.

With reference to figure 2, show the representational snus type tobacco product comprising extract of the present invention.Particularly, Fig. 2 explains the smokeless tobacco product 40 with the permeable outer pouch 42 of water, described outer pouch 42 is equipped with smokeless tobacco composition 44, and wherein said tobacco compositions comprises fragment or the particulate tobacco material of the carrier serving as extract of the present invention.

Many exemplary smokeless tobacco compositions can benefiting from the application of extract of the present invention comprise fragment or particulate tobacco material, and the latter can serve as the carrier of good to eat extract of the present invention.Smokeless tobacco composition of the present invention can also comprise water miscible polymeric adhesive material and other optional composition, and they can provide so soluble composition: it is disintegration lentamente in the oral cavity in use.In certain embodiments, described smokeless tobacco composition can comprise lipid composition, described iipidomic branch be provided in melt in oral cavity can melted composition (be only different from dissolve), such as on August 11st, 2010 submit to and be incorporated to the composition of setting forth in the U. S. application numbers 12/854,342 of the people such as Cantrell herein by reference.

In a specific smokeless tobacco product embodiment, extract of the present invention is added in non-tobacco vegetable material, be such as selected from the vegetable material of potato, beet (such as, sugar beet), cereal, pea, apple etc.Described non-tobacco vegetable material can use with the form through processing.In certain preferred aspects, described non-tobacco vegetable material can use through the form extracted, and like this, to remove in some Solvent soluble components at least partially from this material.The vegetable material of the extraction of non-tobacco is highly extracted usually, this means, a large amount of water-soluble portion of vegetable material is removed.Such as, by extracting a large amount of water-soluble components from vegetable material, the slurry that water extraction is got can be obtained.Such as, the vegetable material that some water extraction is got can comprise and be less than about 20 % by weight, be often less than the water-soluble component of about 10 % by weight; And depend on processing conditions, the vegetable material that some water extraction is got can be substantially free of water-soluble component (such as, being less than the water-soluble component of about 1 % by weight).The vegetable material that a kind of preferred water extraction is got is the sugar beet slurry (the sugar beet leaf that such as, water extraction is got is starched) that water extraction is got.The non-tobacco vegetable material extracted usually with can be described as tear up, grinding, granular, fine particles or powder type use.Non-tobacco vegetable material and the dry weight ratio of tobacco extract of the present invention are generally about 4:1 to about 1:4, about 2:1 to about 1:2, and are often about 1.5:1 to about 1:1.5.The U. S. application of the people such as the Beeson that this kind of smokeless tobacco product was submitted to see on April 8th, 2010 number 12/756,656, it is incorporated to herein by reference.

Other additive can mix with smokeless tobacco composition according to the present invention, or otherwise mixes wherein.Described additive can be man-made additive, or or biogenicly can obtain or derive from herbal medicine.Exemplary additive types comprises: salt (such as, sodium chloride, potassium chloride, natrium citricum, potassium citrate, sodium acetate, potassium acetate etc.), natural sweetener (such as, fructose, sucrose, glucose, maltose, vanillic aldehyde, ethyl vanillin glucoside, mannose, galactolipin, lactose etc.), artificial sweetening agent (such as, Sucralose, asccharin, Aspartame, acesulfame potassium, knob is sweet), organic and inorganic filler (such as, particulate, process particulate, loose particulate, maltodextrin, dextrose, calcium carbonate, calcium phosphate, cornstarch, lactose, sweet mellow wine, xylitol, sorbierite, the cellulose etc. of fine crushing), adhesive (such as, PVP, sodium carboxymethylcellulose and other modified cellulose class adhesive, mosanom, xanthans, starch-based adhesive, gum arabic, lecithin etc.), pH adjusting agent or buffer (such as, metal hydroxides, preferred alkali metal hydroxide, as NaOH and potassium hydroxide, with other alkali metal buffer as metal carbonate, preferred potash or sodium carbonate, or alkali metal bicarbonate salt is as sodium acid carbonate etc.), colouring agent (such as, dyestuff and pigment, comprise burnt sugar coloring and titanium dioxide etc.), NMF (such as, glycerine, propane diols etc.), oral care additives (such as, thyme linaloe oil, eucalyptus oil and zinc), anticorrisive agent (such as, potassium sorbate etc.), syrup (such as, honey, high-fructose corn syrup etc.), disintegration auxiliary agent (such as, microcrystalline cellulose, Ac-Di-Sol, Crospovidone, primojel, pregelatinized com starch etc.), flavor enhancement and seasoning mixture, antioxidant, and composition thereof.If necessary, can by described additive package encapsulated, as described in the U.S. Patent Application Publication No. 2008/0029110 of the people such as Dube, it is incorporated to herein by reference.

The amount adding the tobacco extract in tobacco compositions or tobacco product can change, and partly depends on the desired function of described extract, the chemical component of described extract and add the tobacco compositions of described extract or the type of product wherein.Unless otherwise indicated herein, based on the gross dry weight of tobacco compositions adding described extract wherein, the amount added in tobacco product is no more than about 25 % by weight usually.When described extract is used in smoking product, based on the gross dry weight of the tobacco-containing material in described smoking product, the amount of extract normally at least about 5ppm, usually at least about 10ppm, often at least about 100ppm; But based on the gross dry weight of the tobacco-containing material in described smoking product, be usually less than about 5%, be usually less than about 2%, be often less than about 1%.When described extract is used in smokeless tobacco product, based on the gross dry weight of the tobacco-containing material in described smokeless tobacco product, the amount of extract normally at least about 5ppm, usually at least about 10ppm, often at least about 100ppm; But based on the gross dry weight of the tobacco-containing material in described smokeless tobacco product, be usually less than about 10%, be usually less than about 5%, be often less than about 1%.

Experimental section

The following example explains aspect of the present invention more fully, and setting forth described embodiment is to illustrate some aspect of the present invention, and is not interpreted as its restriction.Unless otherwise noted, all numbers and percents by weight.

embodiment 1

Water extraction fire of learning from else's experience is used to toast tobacco.Typical leaching process at the temperature of about 72 DEG C by the tobacco of pulverizing (such as, 100% through 0.250 inch of sieve) with water with 8 parts of water: the ratio of 1 portion of tobacco mixes.Described mixture is stirred 1 hour, and is filtered by use 5 micron filter bag, the solid that removing suspends.The tobacco extract obtained retains the fragrance and sense quality that toast tobacco through fire.Original toasting tobacco through fire had the BaP level of about 150 to 800ppb before extracting, and the liquid extract of separation has the BaP level being less than about 1ppb.

embodiment 2

The leaching process identical with described in embodiment 1 is carried out to the tobacco of drying.The original tobacco of drying had the BaP level of about 10-150ppb before extracting, and the liquid extract of separation has the BaP level being less than about 1ppb.

embodiment 3

Use supercritical CO ₂extract have 10% water content grind toast tobacco through fire.An exemplary leaching process adopts Jasco supercritical fluid extraction system, it comprises preparation pump, post thermostat, photodiode array detector, HPLC pump, automatically back pressure regulator and 6 valve change unit, and described 6 valve change unit can collect sample in time sequencing mode in single-trial extraction running.Stainless steel pressure extraction vessel is positioned at post thermostat, has the pressure limit of 40MPa.Use 100%CO ₂extract, and use methyl alcohol to trap the compound of extraction as backflow.

Change and adopt it to carry out pressure, temperature and the CO extracted ₂flow velocity, to assess separately the impact of B [a] p and TSNA from the removing of tobacco.Pressure is remained on 10,20 or 30MPa, at temperature being remained on 40 DEG C or 60 DEG C, and by CO ₂flow rate set is 5 or 10mL/min.The solid residue hexane class obtained is extracted, and carries out liquid chromatography, with B [a] p and the TSNA concentration of the material extracted relative to the analog value evaluation of undrawn tobacco.

Under higher temperature and lower pressure, only observe the little minimizing of B [a] p (~ 5% reduces) and TSNA (being less than about 20% to reduce).The pressure carrying out extracting under being increased in it can provide suitable result.Use medium (20MPa) pressure, the temperature of 60 DEG C and the flow velocity of 10mL/min, obtain the highest TSNA and reduce.Use the pressure of 30MPa, the temperature of 60 DEG C and the flow velocity of 10mL/min, obtain the highest B [a] p and reduce (62% reduces).

embodiment 4

Use the method described in embodiment 3, use supercritical CO ₂the water extraction extracting the water content with 11% get through fiery flue-cured tobacco straw pulp.By CO ₂temperature, at 10mL/min, is set in 40 DEG C or 60 DEG C by flow rate set, and by pressure setting 10,20 or 30MPa, with the impact on the removing toasted tobacco through fire that B [a] p and TSNA gets from water extraction of evaluation temperature and pressure.

Along with temperature and pressure increases, remove more B [a] p and TSNA from tobacco.But, at the pressure of 10MPa, make temperature be increased to 60 DEG C from 40 DEG C, on the removing toasted tobacco through fire that B [a] p or TSNA gets from water extraction, not there is a lot of impact.Use the pressure of 30MPa and the temperature of 60 DEG C, obtain the highest TSNA and reduce (63%).Use the temperature of the pressure of 30MPa and 40 DEG C or 60 DEG C, obtain the highest B [a] p and reduce (being 46% and 47% respectively).

embodiment 5

As described in embodiment 3, use supercritical CO ₂extract have 10% water content grind toast tobacco through fire.Under pressure is remained on 20MPa, at temperature being remained on 40 DEG C, and flow velocity is remained on 10mL/min CO ₂.Change extraction time to assess the impact of extraction time on the removing of B [a] p and TSNA.The period lasting 15 minutes, 30 minutes, 45 minutes, 60 minutes and 120 minutes extracts.With the extraction sample observation of 30 minutes to the minimizing of B [a] p and TSNA suitable with the minimizing of arriving with the sample observation extracted more than 30 minutes; Therefore, 30 minutes are selected as the extraction duration of other experiment.

Use different extraction times, extract similarly have that the water extraction of the water content of 11% gets through fiery flue-cured tobacco straw pulp.The extraction time of 30 minutes causes the abundant removing of B [a] p and TSNA again.

embodiment 6

As described in embodiment 3, use supercritical CO ₂the tobacco pulp sample roasting through fire got with water extraction extracting that each bakes through fire.Change the water content of tobacco sample before extracting, to evaluate the impact of moisture on the removing of B [a] p and TSNA.Under pressure is remained on 20MPa, at temperature being remained on 40 DEG C, flow velocity is 10mL/min CO ₂, running time is 30 minutes.Before extraction, the moisture of varying level is added to tobacco sample, to obtain having toasting tobacco sample and toasting tobacco sample through fire of having that the water extraction of 10%, 11%, 16%, 21% and 27% water content gets through fire of 10%, 16%, 21%, 25% and 31% water content.Calculate the actual amount of the tobacco sample loaded in extraction vessel based on water content, to reach the oven-dry weight of identical amount (10g), make the tobacco of each sample carrying out extracting at first containing identical total amount.Each sample is extracted, and by air-dry at least 4 days of the solid residue that obtains, with the level making the water content of each sample residue reach relatively identical.

Toast tobacco for through fire, make water content be increased to 31% from 10% and cause larger TSNA to reduce (80%TSNA when being reduced in 31% water content from the 60%TSNA when 10% water content reduces) and larger B [a] p minimizing (80%B [a] p when being reduced in 31% water content from 45%B [a] p during in 10% water content reduces).

That gets for water extraction toasts tobacco through fire, makes water content be increased to 27% from 10% and causes larger TSNA to reduce (80%TSNA when 45%TSNA when 10% water content is reduced in 27% water content reduces) and larger B [a] p minimizing (50%B [a] p when 20%B [a] p during in 10% water content is reduced in 27% water content reduces) similarly.

In appearance, moisture can promote the removing of B [a] p and TSNA to the introducing of tobacco-containing material.Although be not intended to become restriction of the present invention, a kind of explanation is, water add the internal structure can opening tobacco, make it more can be extracted close.Another kind of explanation is, because B [a] p is nonpolar, the existence of more water in tobacco can more effectively by B [a] p " release " tobacco.TSNA has polarity with nonpolar feature, and thus, this theory can explain that B [a] p and TSNA removes to be increased along with tobacco moisture level and increase.

embodiment 7

As described in embodiment 3, use supercritical CO ₂the tobacco pulp sample roasting through fire got with water extraction extracting that each bakes through fire.Add the ethanol of different amount to serve as supercritical CO ₂conditioning agent, to evaluate the impact of ethanol on the removing of B [a] p and TSNA.Also change temperature and pressure to evaluate the impact of these parameters when being added in extraction system by ethanol.

Pressure is remained on 10 or 20MPa, at temperature being remained on 40 DEG C or 60 DEG C, flow velocity is 10mL/min CO ₂, running time is 30 minutes.The ethanol of difference amount is added the CO for carrying out tobacco sample extraction ₂in.Particularly, the Extraction medium of evaluation is: 100%CO ₂, the CO containing 10 % by weight ethanol ₂, and the CO containing 30 volume % ethanol ₂.

That water extraction is got and the tobacco baked through fire and the extraction toasted tobacco through fire is carried out by each in these Extraction medium.At the temperature of 40 DEG C and 60 DEG C and the pressure at 10MPa to 20MPa, extract with often kind of Extraction medium.Extract often kind of sample, and evaluate the solid residue obtained, to determine the minimizing of B [a] p and TSNA.For toasting tobacco through fire of toasting tobacco through fire and get with water extraction, under all temperature and pressures evaluated regulate, add the larger minimizing that ethanol can cause B [a] p and TSNA.

Such as, under 60 DEG C and 10MPa, with independent CO ₂the extraction toasted tobacco through fire of getting water extraction causes 20% of B [a] p to reduce and 32% the reducing of TSNA, and with containing the CO of 30% ethanol ₂extraction cause B [a] p 71% reduce and TSNA 79% minimizing.Under the same conditions, with independent CO ₂37% minimizing of B [a] p and 46% of TSNA is caused to reduce to the extraction toasted tobacco through fire, and with containing the CO of 30% ethanol ₂extraction cause B [a] p 80% reduce and TSNA 75% minimizing.

Under the pressure of the temperature of 60 DEG C and 20MPa, with the CO containing 30% ethanol ₂extraction medium reach the highest B [a] p in fire toasts tobacco that water extraction in this embodiment gets and reduce level (74%).The temperature of 60 DEG C and 10 or 20MPa pressure under, with containing the CO of 30% ethanol ₂extraction medium reach the highest TSNA minimizing level (79%) in fire toasts tobacco that water extraction in this embodiment gets.

Under the pressure of the temperature of 60 DEG C and 10MPa, with the CO containing 30% ethanol ₂extraction medium reach the highest B [a] p in this embodiment in fire toasts tobacco and reduce level (80%).Under the pressure of the temperature of 60 DEG C and 10MPa, with the CO containing 30% ethanol ₂extraction medium reach the highest TSNA minimizing level (75%) in this embodiment in fire toasts tobacco.

Usually, the ethanol of about 30 volume % is at the most added the CO as Extraction medium ₂the middle removing that can increase B [a] P and TSNA.The temperature of such extraction is changed to 60 DEG C from 40 DEG C almost do not act on, although in some cases, it can cause B [a] P and TSNA strengthened a little to remove.Similarly, the pressure of such extraction is increased to 20MPa from 10MPa and does not almost act on, although in some cases, it can cause B [a] P and TSNA strengthened a little to remove.

The those skilled in the art in the invention with the instruction benefit provided in the foregoing written description will expect many amendments of the present invention and other embodiment.Therefore, should be appreciated that and the invention is not restricted to disclosed specific embodiments, and amendment and other embodiment are intended to be included within the scope of the appended claims.Although there is used herein concrete term, they only use with general and descriptive implication, and are not used in the object of restriction.

Claims

1. production is used in a method for the tobacco compositions in tobacco product, and the feature of described tobacco compositions is benzo [a] the pyrene concentration reduced, and described method comprises:

The slurry through extracting through baking tobacco-containing material will with the first benzo [a] pyrene concentration mixes with supercritical carbon dioxide, to provide the intimate contact between the described slurry through extraction and described supercritical carbon dioxide;

Maintain described intimate contact certain hour at a certain temperature, described temperature and time is enough to the treated tobacco pulp that formation shows the second benzo [a] the pyrene concentration lower than described first benzo [a] pyrene concentration; With

Be separated with remaining supercritical carbon dioxide extract by described treated tobacco pulp, described remaining supercritical carbon dioxide extract comprises the component of the described tobacco-containing material dissolved in described supercritical carbon dioxide.

2. method according to claim 1, the wherein said slurry through extracting comprise through baking tobacco-containing material toasting tobacco through fire of grinding.

3. method according to claim 2, the wherein said slurry through extracting is the tobacco-containing material that water-based is extracted.

4. method according to claim 1, the pressure wherein carrying out described mixing under it is about 10MPa or larger.

5. method according to claim 1, the pressure wherein carrying out described mixing under it is about 20MPa or larger.

6. method according to claim 1, the pressure wherein carrying out described mixing under it is to about between 40MPa at about 10MPa.

7. method according to claim 1, the temperature of wherein carrying out described mixing under it is about 40 DEG C or larger.

8. method according to claim 1, the temperature of wherein carrying out described mixing under it is about 50 DEG C or larger.

9. method according to claim 1, the temperature of wherein carrying out described mixing under it is between about 40 DEG C to about 60 DEG C.

10. method according to claim 1, the wherein said row that is mixed into was at least about period of 15 minutes.

11. methods according to claim 1, the wherein said row that is mixed into was at least about period of 30 minutes.

12. methods according to claim 1, wherein said blend step comprises: mixed with supercritical carbon dioxide and ethanol by the described slurry through extracting.

13. methods according to claim 12, wherein said ethanol exists with the amount of the stereometer about 10% to about 30% of described supercritical carbon dioxide and ethanol.

14. methods according to claim 1, wherein said first benzo [a] pyrene concentration is at least about 200ng/g, and described second benzo [a] pyrene concentration is less than about 80ng/g.

15. methods according to claim 1, the TSNA concentration of wherein said treated tobacco pulp is less than the TSNA concentration of the described slurry through extracting through baking tobacco-containing material.

16. methods according to claim 15, the wherein said slurry through extracting through baking tobacco-containing material has the TSNA concentration being greater than about 5,000ng/g, and described treated tobacco pulp has the TSNA concentration being less than about 2,000ng/g.

17. methods according to claim 1, described method also comprises: added by tobacco extract in described treated tobacco pulp to form tobacco compositions.

18. methods according to claim 17, wherein said tobacco extract is aqueous extract.

19. methods according to claim 17, wherein said tobacco extract and described treated tobacco pulp are derived from identical tobacco sample.

20. methods according to claim 1, comprising through baking tobacco-containing material of the wherein said slurry through extracting to toast tobacco material through fire, and wherein said method also comprises and water-based being added in described treated tobacco pulp to form tobacco compositions through the fire extract that toasts tobacco.

21. methods according to any one in claim 1-20, described method also comprises: introduced in tobacco product by described treated tobacco pulp.

22. methods according to claim 21, wherein said tobacco product is selected from: smoking product, smokeless tobacco product and the aerocolloidal device of generation for the vegetable material structure that do not burn.

23. methods according to claim 21, wherein said tobacco product is selected from following smokeless tobacco composition: wet snuff, dry snuff, chewing tobacco, containing the chewing gum of tobacco and soluble or fusible tobacco product.

24. 1 kinds of tobacco products of slurry through extracting comprised through baking tobacco-containing material, the wherein said slurry through extracting through baking tobacco-containing material is characterized as being B [a] the p concentration having and be less than about 80ng/g.

25. tobacco products according to claim 24, the wherein said slurry through extracting is characterized as being the TSNA concentration having and be less than about 2,000ng/g.

26. tobacco products according to claim 24, described tobacco product also comprises the tobacco extract carried by the described slurry through extracting.

27. tobacco products according to claim 26, wherein said tobacco extract is aqueous extract.

28. tobacco products according to claim 26, wherein said tobacco extract and the described slurry through extracting through baking tobacco-containing material are derived from identical tobacco sample.

29. tobacco products according to claim 24, comprising through baking tobacco-containing material of the wherein said slurry through extracting to toast tobacco material through fire, and wherein said tobacco product also comprises the water-based of being carried by the described slurry through extracting to toast tobacco extract through fire.

30. tobacco products according to claim 24, wherein said tobacco product is in following form: smokeless tobacco composition, smoking product or the aerocolloidal device of generation for the vegetable material structure that do not burn.

31. tobacco products according to claim 30, wherein said tobacco product is the form in being selected from following smokeless tobacco composition: wet snuff, dry snuff, chewing tobacco, containing the chewing gum of tobacco and soluble or fusible tobacco product.