TWI428093B - 煙草組合物(二) - Google Patents
煙草組合物(二) Download PDFInfo
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B13/00—Tobacco for pipes, for cigars, e.g. cigar inserts, or for cigarettes; Chewing tobacco; Snuff
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/70—Fixation, conservation, or encapsulation of flavouring agents
- A23L27/79—Fixation, conservation, or encapsulation of flavouring agents in the form of films
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/81—Solanaceae (Potato family), e.g. tobacco, nightshade, tomato, belladonna, capsicum or jimsonweed
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Description
本發明係關於煙草產品之領域。
無煙菸草因不需燃燒而廣受大眾喜愛。無煙菸草的型式包括咀嚼菸草(chewing tobacco)、乾鼻煙(dry snuff)及濕鼻煙(moisture snuff)。一般來說,上述各種的無煙菸草皆是利用以下無特別順序的步驟製備:切割及研磨菸草至一適當的大小;將菸草以一溶液浸泡或噴灑;部份地進行乾燥;將菸草置於容器中一段時間;以及包裝。
咀嚼菸草一般包括三種型式:“口嚼(plug)”,將菸草壓成任何形狀;扭煙(twists),將菸葉纏繞至繩索狀;散狀(loose)、葉狀(leafy)咀嚼菸草,將菸草置於一類似封套狀的容器中。口嚼菸草通常含有15%體積百分比或更少的水份,以形成較硬的口嚼菸草,而水份高於15%體積百分比則可形成較軟的口嚼菸草。扭煙及散煙所含的水份通常較少。
鼻煙(snuffs)包括乾式或濕式。乾鼻煙通常含有約8%的水份。濕鼻煙通常具有40%至60%的水份,且可依不同的產品產生不同的大小。
本發明提供煙草組合物與其用途及製造方法。本發明組合物基於多種技術。技術包括薄膜物、錠劑、形狀化部件、膠、可吞食之單位、不溶基質與中空形狀物。除煙草外,組合物亦可含有調味劑、著色劑及本說明書中所述之其他添加物。組合物亦可為口中可崩解者。本說明書詳細說明例示組合物及其製
造方法。
例如,述於本文之任何組合物可包括調味劑或調味遮蔽劑。例示調味劑包括:甘草(licorice)、葛根(kudzu)、八仙花(hydrangea)、日本白皮木蘭葉(Japanese white bark magnolia leaf)、洋甘菊(chamomile)、胡蘆巴(fenugreek)、丁香(clove)、薄荷腦(menthol)、日本薄荷(Japanese mint),洋茴香(aniseed)、肉桂(cinnamon)、草本植物(herb)、冬青(wintergreen)、櫻桃(cherry)、莓果(berry)、蘋果、蜜桃、再蒸餾之威士忌酒(Dramboui)、波本酒(bourbon)、蘇格蘭威士忌(scotch)、威士忌、綠薄荷(spearmint)、薄荷(peppermint)、薰衣草(lavender)、小荳蔻(cardamon)、旱芹(apium graveolens)、香苦木(cascarilla)、荳蔻(nutmeg)、檀香(sandalwood)、佛手柑(bergamot)、天竺葵(geranium)、蜂蜜精油(honey essence)、玫瑰油(rose oil)、香草(vanilla)、檸檬油(lemon oil)、柑橘油(orange oil)、阿勃勒(cassia)(桂皮)、香柏木(caraway)、干邑酒(cognac)、茉莉(jasmin)、山楂(ilangilang)、鼠尾草(sage)、茴香(fennel)、甜椒(piment)、薑(ginger)、八角(anise)、胡荽(coriander)、咖啡(coffee)、或薄荷屬內任一種之薄荷油。
本發明之任何組合物亦可包括甜味劑(如蔗糖、蔗糖素(sucralose)、乙醯磺胺酸鉀(acesulfame potassium)、阿斯巴甜、甜精(saccharine)、糖精(cyclamates)、乳糖、葡萄糖、果糖、山梨醇、甘露醇);界面活性劑;增塑劑(如甘油、丙二醇、聚乙二醇、山梨醇/甘露醇、乙醯化一甘油酯、三乙酸酯、1,3-丁二醇);填充劑(如澱粉、微結晶纖維素、木漿、可溶性纖維、碳酸鈣、磷酸二鈣、硫酸鈣與粘土);潤滑劑(如硬脂酸與硬脂酸酯)或蠟(如卵磷脂、單硬脂酸甘油酯、單硬脂酸聚乙二醇酯);防腐劑(如羥基苯甲酸甲酯(methyl paraben)、山梨
酸鉀)及/或安定劑(如維生素C、單類黃酮檸檬酸酯、BHT與BHA)。
本文所述之任何組合物可進一步包括塗覆,如無光澤的或光亮的。該塗覆較佳的包括著色劑、調味劑、甜味劑或者調味遮蔽劑。該塗覆亦可包括與組合物之配方(format)不同的調味、著色劑或者崩解速率。塗覆亦可包括煙草。
本文所述之任何組合物更可包括印製圖案,如標誌圖案。印製圖案可包括著色劑、煙草、調味劑、甜味劑或者調味遮蔽劑。本文描述的任何組合物表面亦可包括浮雕圖案(a pattern in relief)。
包括於任何組合物之煙草可為粉狀、粒狀、條狀或為可溶於口中的形式。
本文所述之任何組合物更可包括片狀,例如含有煙草或各種調味劑或著色劑。
本文所述之任何組合物可製成適於口服的形狀。本發明之組合物更可提供煙草的滿足感,例如,超過10秒至30分鐘期間。
本發明亦提供藉由置放本文所述之任何組合物的至少一部分於口中以獲得煙草滿足感的方法。
本發明亦提供製造本發明之組合物的方法。任何該等方法更可包括組合物添加塗覆至組合物,如藉由噴灑、刷塗、輥塗、刮柄澆鑄、狹槽塗覆、突起塗覆或者熱溶析出。任何該等方法亦可包括在組合物印製圖案,如藉由膠印法、彈性凸版印製油墨法、凹版印製法、噴墨法、雷射或掃描列印法。此外,製造組合物的方法亦可包括將調味劑、調味遮蔽劑或者其他本所述之成份添加至其配方或組合物。
本發明中「配方(format)」,如本文所提供者,意指組合物中的成分或成分編集物,如載劑或試劑。
「煙草」是指煙草屬Nicotiana之任何植物成員之任何部
份,例如葉、花、根和莖。典型的煙草種類包括黃花煙草(N.rustica)與紅花煙草(N.tabacum)(如LA B21、LN KY171、TI 1406、巴斯托馬煙草(Basma)、南美涼(晾)煙型煙草(Galpao)、波力克煙草(Perique)、雪茄煙品系(Beinhart 1000-1與Petico)。其他種類包括顯脈煙草(N.acaulis)、尖葉煙草(N.acuminata)、多花種尖葉煙草(N.acuminata var.multiflora)、非洲煙草(N.africana)、花煙草(N.alata)、抱莖煙草(N.amplexicaulis)、阿瑞特希煙草(N.arentsii)、斑點煙草(N.attenuate)、班納威第希煙草(N.benavidesii)、本塞姆氏煙草(N.benthamiana)、畢格羅夫煙草(N.bigelovii)、玻那雷恩煙草(N.bonariensis)、穴居煙草(N.cavicola)、克利夫蘭煙草(N.clevelandii)、心葉煙草(N.cordifolia)、紫花煙草(N.corymbosa)、德氏煙草(N.debneyi)、木絲煙草(N.excelsior)、長葉煙草(N.forgetiana)、飄香煙草(N.fragrans)、粉藍煙草(N.glauca)、黏毛煙草(N.glutinosa)、顧德斯比第煙草(N.goodspeedii)、金翅煙草(N.gossei)、後綴煙草(N.hybrid)、黑煙草(N.ingulba)、川上氏煙草(N.kawakamii)、騎士煙草(N.knightiana)、大葉煙草(N.langsdorffii)、線狀煙草(N.linearis)、長花煙草(N.longiflora)、濱海煙草(N.maritime)、巨虹吸煙草(N.megalosiphon)、米爾希煙草(N.miersii)、夜花煙草(N.noctiflora)、裸莖煙草(N.nudicaulis)、鈍圓煙草(N.obtusifolia)、西方煙草(N.occidentalis)、香芥亞種西方煙草(N.occidentalis subsp.hesperis)、耳狀煙草(N.otophora)、鬚齒煙草(N.paniculata)、少花煙草(N.pauciflora)、碧冬煙草(N.petunioides)、藍茉莉葉煙草(N.plumbaginifolia)、四齒煙草(N.quadrivalvis)、雷蒙氏煙草(N.raimondii)、波紋煙
草(N.repanda)、姜鮫煙草(N.rosulata)、黑亞種姜鮫煙草(N.rosulata subsp.Ingulba)、圓葉煙草(N.rotundifolia)、鼓苞煙草(N.setchellii)、模仿煙草(N.simulans)、單葉煙草(N.solanifolia)、紫煙草(N.spegazzinii)、史塔克托尼煙草(N.stocktonii)、香甜煙草(N.suaveolens)、美花煙草(N.sylvestris)、球花煙草(N.thyrsiflora)、絨毛煙草(N.tomentosa)、絨毛狀煙草(N.tomentosiformis)、沙漠煙草(N.trigonophylla)、傘型煙草(N.umbratica)、波狀煙草(N.undulate)、絨葉煙草(N.velutina)、威甘地奧蒂絲煙草(N.wigandioides)、與花煙草(N.x sanderae)。煙草可為完整的、經切絲的、經切割的、經卷曲的、經熟成(aged)的、經醱酵的或經其他處理程序,如顆粒化或經包埋。煙草亦可為完工產品形式,包括但不限於任何口服的非易燃煙草,如無煙煙草。該無煙的煙草包括吸入(濕或乾)、咀嚼煙草、鬆散煙草、袋狀煙草等,或含於本文之任何形式。此名詞亦包括二種或二種以上感官察覺成份(organoleptic components)的煙草萃取物。
「煙草的滿足感」一詞意指有關煙草感官察覺成分及當使用無煙煙草於口中釋放出添加之調味成分所相關之經驗。選擇使用無煙煙草的成年消費者會依其個別的偏好,這些偏好包括,不限於調味、煙草切片、形式、使用方便性及包裝方式,而購買無煙煙草產品。
「感官察覺」一詞意指關於或有助於消費者整體感覺的認知,包括如香氣、香味、調味、味覺、味道、口感等組合。
「非易燃」一詞意指在一般用途不會燃燒。
本發明之組合物於尺寸、使用方便性及經控制的崩解速率的觀點具有優勢。
除非特別說明,所有的百分比為重量百分比。
其他特徵及優勢將由以下說明及申請專利範圍而更為顯明。
本發明提供一般用於煙草滿足感之煙草組合物。
有用於本發明之組合物之煙草包括任何原始未加工或經加工形式,如粉狀、粒狀、或絲狀。較佳地,煙草是尺寸化製成崩解於口(如溶解),給予可溶解的感覺(如煙草在口腔中沒有實體感),或易於吞食。或者,煙草可尺寸化或製成在口中提供有實體感的經驗。代表性的平均尺寸在1至1000微米的範圍內,例如:約800、500、250、100、80、75、50、25、20、15、10、8、6、5、3、2或1微米,或更小,以80微米或更小為佳。煙草組合物亦可為漿狀或可流動膠形式。可流動膠意指將溶解於水之配方與煙草混合之混合物,再與易混合溶劑混合而預防配方之完全解體。該混合物引起該配方膨脹而形成黏糊,該黏糊為仿塑膠狀,且受微壓後可易於由容器(如筒管)中分裝。煙草的實施例是無煙煙草。進一步的煙草揭示於美國專利公開號2003/0094182與2003/0070687,U.S.S.N.60/603,887及2004年11月5日申請,名稱為「煙草組合物」之U.S.S.N.10/981,948;其所揭示內容合併於此作為參考文獻。本組合物所使用的煙草亦可根據美國專利公開號2004/0112394所揭示的方法來製備;其所揭示內容合併於此作為參考文獻。其他適合的煙草已知於此項技術中。
煙草成分可隨意的或均勻的分布於組合物中,或是濃縮於其各種區域,如中心或表面。
取決於所需特性及組合物的最終用途,典型的最終煙草濃度範圍為最終組合物之1至99重量%,例如最多10、15、20、25、
30、35、40、45、50、55、60、65、70、75、80、85、或90%。較佳的具體例中,組合物包括約25%煙草。
一般而言,本發明之組合物是用於口服用途或消費的。含有煙草之組合物可製成任何適合口部相容的方式。煙草可直接與該配方混合或由該形式所支持。舉例而言,組合物可含有煙草,如經乾燥顆料、細絲、粒狀、粉末或漿狀,採取置放、混合、包圍或其他組合配方。組合物中煙草可為或可不為,或經理解為可溶的。一具體例中,組合物為較少噴出火花之煙草組合物。組合物亦可包括菸草之形式或類型的混合物。組合物可為發泡式或稠密的。發泡式的組合物可為堅硬的或撓性的,且可為水溶性、水不溶性或熱塑性的配方。例示組合物經敘述於本文。一具體例中,本發明之組合物為不可燃的。
適用於本發明組合物之配方包括口服相容聚合物,如纖維素(如羧甲基纖維素(CMC)、羥丙基纖維素(HPC)、羥乙基纖維素(HEC)、羥丙基甲基纖維素(HPMC)及甲基纖維素(MC))、天然聚合物(如澱粉及改質澱粉、蒟蒻、膠原蛋白、菊芋多醣(inulin)、黃豆蛋白質、乳清蛋白、酪蛋白及小麥麩)、海藻衍生聚合物(如角叉菜膠(卡帕(kappa)、依而他(iota)及倫巴(lambda))、海藻膠(alginates)及海藻酸丙二醇酯)、微生物衍生聚合物(如黃原膠(xanthan)、右旋膠(dextran)、普路蘭膠(pullulan)、熱凝膠(curdlan)和結冷膠(gellan gum))、萃取物(如刺槐豆膠(locust bean gum)、瓜爾豆膠(guar gum)、他拉膠(tara gum)、黃耆膠(gum tragacanth)、果膠(低甲氧基及經醯胺化)、洋菜、玉米醇溶蛋白(zein)、卡拉牙膠(karaya)、明膠、洋車前子(psyllium seed)、幾丁質及幾丁醣)、滲出液(如阿拉伯樹脂及蟲膠)、合成高分子材料(如聚乙烯吡咯烷酮、聚環氧乙烷及聚乙烯醇)。其它在此項技術上已
知具實際用途的配方,舉例而言,如參閱(Krochta等人)Food Technology,1997,51:61-74,Gilicksman Food Hydrocolloids CRC 1982,Krochta Edible Coatings and Films to Improve Food Quality Technomic 1994,Industrial Gums Academic 1993,Nussinovitch Water-Soluble Polymer Applications in Foods Blackwell Science 2003。根據所需特性,組合物亦可含有填充物(如澱粉、微晶纖維素、木質紙漿(如International Fibers公司生產的純木質纖維,Solkafloc)、可溶性纖維(如Matsushita公司生產的水溶性膳食纖維,Fibersol)、碳酸鈣、磷酸二鈣、硫酸鈣與粘土)、潤滑劑(如卵磷脂、硬脂酸、硬脂酸鹽(如鎂/鉀),與蠟質(如單硬脂酸甘油酯、硬脂酸聚乙二醇酯及乙醯化單甘油脂))、增塑劑(如甘油、丙二醇、聚乙二醇、山梨醇/甘露醇、三乙酸酯、1,3-丁二醇)、安定劑(如維生素C、單類黃酮檸檬酸酯、BHT、BHA)、或其他化合物(如植物油、界面活性劑與防腐劑)。有些化合物兼具增塑劑與潤滑劑的功能。
本發明之組合物可含有調味劑萃取物(如甘草(licorice)、葛根(kudzu)、八仙花(hydrangea)、日本白皮木蘭葉(Japanese white bark magnolia leaf)、洋甘菊(chamomile)、胡蘆巴(fenugreek)、丁香(clove)、薄荷腦(menthol)、日本薄荷(Japanese mint),洋茴香(aniseed)、肉桂(cinnamon)、草本植物(herb)、冬青(wintergreen)、櫻桃(cherry)、莓果(berry)、蘋果、蜜桃、再蒸餾之威士忌酒(Dramboui)、波本酒(bourbon)、蘇格蘭威士忌(scotch)、威士忌、綠薄荷(spearmint)、薄荷(peppermint)、薰衣草(lavender)、小荳蔻(cardamon)、旱芹(apium graveolens)、香苦木(cascarilla)、荳蔻(nutmeg)、檀香(sandalwood)、佛手柑(bergamot)、天竺葵(geranium)、蜂蜜精油(honey
essence)、玫瑰油(rose oil)、香草(vanilla)、檸檬油(lemon oil)、柑橘油(orange oil)、阿勃勒(cassia)(桂皮)、香柏木(caraway)、干邑酒(cognac)、茉莉(jasmin)、山楂(ilangilang)、鼠尾草(sage)、茴香(fennel)、甜椒(piment)、薑(ginger)、八角(anise)、胡荽(coriander)、咖啡(coffee)、或薄荷屬內任一種之薄荷油)、調味遮蔽劑、苦味受體位置阻斷劑、受體位置強化劑、甜味劑(如蔗糖素、乙醯磺胺酸鉀(acesulfame potassium,Ace-K)、阿斯巴甜、甜精、糖精、乳糖、葡萄糖、果糖、山梨醇、甘露醇)、及其他所需添加劑如葉綠素、礦材料、植物性藥材或者口氣清新劑。
調味劑也可由植物材料供給,如薄荷葉,其一般具有10%調味劑油及90%不可溶纖維。例示植物更包括甘草(licorice)、葛根(kudzu)、八仙花(hydrangea)、日本白皮木蘭葉(Japanese white bark magnolia leaf)、洋甘菊(chamomile)、胡蘆巴(fenugreek)、丁香(clove)、日本薄荷(Japanese mint),肉桂(cinnamon)、草本植物(herb)、櫻桃(cherry)、莓果(berry)、蘋果、蜜桃、薰衣草(lavender)、小荳蔻(cardamon)、旱芹(apium graveolens)、香苦木(cascarilla)、荳蔻(nutmeg)、檀香(sandalwood)、佛手柑(bergamot)、天竺葵(geranium)、玫瑰(rose)、香草(vanilla)、檸檬(lemon)、柑橘(orange)、阿勃勒(cassia)(桂皮)、香柏木(caraway)、茉莉(jasmin)、山楂(ilangilang)、鼠尾草(sage)、茴香(fennel)、甜椒(piment)、薑(ginger)、八角(anise)、胡荽(coriander)、咖啡(coffee)、或薄荷屬內任一種之薄荷油。
本發明之組合物的調味劑可為調味萃取液、植物材料或其組合。除天然的成分或調味萃取液外,調味劑亦可由模仿性、合成或人造的調味劑成分或含該等成分之混合物提供。調味劑
添加方式可為粉末、油狀物或以包埋的形式。
一些具體例中,組合物於口中崩解。組合物崩解率之範圍可變化於60分鐘至小於1分鐘。快速釋放組合物典型地可於2分鐘內崩解,最佳在1分鐘內或更少的時間,如少於60秒、50秒、45秒、40秒、35秒、30秒、25秒、20秒、15秒、10秒、5秒、4秒、3秒、2秒或1秒。崩解會因任何機制而發生,例如溶解、融化、機械性的崩裂(如咀嚼)、酵素或其他化學性降解或配方與煙草交互作用的崩裂。配方或煙草本身會同樣地崩解。組合物崩解所需之時間由組合物厚度所控制並取決於配方、其他添加劑與使用方式的種類。當放置在口中,組合物可暫時粘附部分的口腔黏膜。此外,煙草滿足感的時間長短不一。時間長度可為組合物崩解率、從組合物感官察覺成分的萃取率及組合物停留在口中的時間所影響到。煙草滿足感可達至少10秒、30秒、45秒、1分鐘、2分鐘、3分鐘、5分鐘、10分鐘、15分鐘、30分鐘或1小時,較佳為從10秒到10分鐘,最佳為從30秒到5分鐘。
於其他具體例中,組合物停留在口中的期間不會崩解。該等組合物中,煙草感官察覺成分之導入口中乃藉著崩解、過濾、萃取或因咀嚼造成之機械性崩裂而發生。
各個組合物的尺寸可為完全符合在口中,或是其可尺寸化為僅符合部分在口中。組合物之較佳截面包括,但不限於,正方形、圓形、長方形、橢圓形、卵形等。較佳的長度會依服用尺寸及成分而不同。通常,最大單一服用份量的尺寸是5公分或更小。或者,煙草產品可製成較大形式,以切開或其他方式分開,如咀嚼、撕裂或在口中崩解等方式供應個別用量。舉例而言,細長條或其他長塊可放置在容器中,由消費者取出所需的用量。較大組合物(或口中部份接連於把手)也可部份插在口中,相似於牙籤或紙捲煙,供消費者吸入或咀嚼。一具體例中,
較大塊可在口中崩解且在一段期間後可完全服用。
薄膜-本發明之組合物可形成口中可崩解之薄膜。該等薄膜可包含單層或多層薄膜。單層薄膜包含煙草、配方與其他成分(如為均質混合物)。多層薄膜可包括含有煙草的數層,例如由相同或不同種類或尺寸的煙草,例如可溶的煙草。多層薄膜可一起積層(laminated)。此外,多層薄膜可含有一層或一層以上的煙草及含有本文所述之添加成分之其他層。舉例而言,個別層可為了調味、甜味、著色劑、崩解率或安定性(如在取用或服用時)而添加。煙草也可以三明治的方式置於2層或更多層之間。三明治之一層或更多層亦可含有煙草。具多層的薄膜中,每層薄膜可以相同或不同的速率崩解,或有在口中不會崩解之層。當崩解速度不同時,組合物可基於層崩解而在不同師兼提供煙草。在多層薄膜中的單層薄膜或個別層也可以經發泡化或充氣方式以供給所需物理特質或所需的溶解或崩解速率。
薄膜可以個別用量尺寸化為符合口中大小。或者,較大的薄膜可由可分開之個別用量製成。舉例而言,薄膜可經包裹或其他方式成形、形成空心管或吸管,其中可以填滿添加成分。此外,本發明的薄膜可製造為,基於乾重,含有高百分比範圍1%至99%的煙草,且可用以製造成薄片或粉末狀以添加在其他組合物。較佳的薄膜厚度典型地為小於1毫米,如小於500、200、100、50、40、30、20、10、5、4、3、2或1微米;較佳為5至125微米。
可使用此項技術中已知之各種方法以製造薄膜。使用的技術可取決於使用於薄膜的配方。例示方法包括溶液鑄造或壓出製造法、熔融擠壓成形(melt extrusion)、滾筒乾燥(drum drying)及輪壓法(calendaring)。一旦成形,薄膜可經改質,如印製或其他塗覆或裝飾薄膜表面。經由印製、塗覆或裝飾加
工,薄膜表面可添加調味劑、著色劑或煙草。目前此項技術上已知的所有印製程序可採用,如膠印(offset)、彈性凸版印製油墨(flexographic)、凹版印製(gravure)、噴墨(ink jet)、雷射(laser)、掃描印製(screen printing)或其他一般的方法。塗覆或裝飾圖案可使用此項技術上已知加工應用在薄膜表面,如噴灑法(spraying)、刷布法(brushing)、翻滾塗覆法(roll coating)、刮柄澆鑄法(doctor bar casting)、狹槽塗覆法(slot coating)、突起塗覆法(extrusion coating)、熱容析出法(hot melt deposition)、存放顆粒(depositing particles)或薄片(flakes)及其他典型的方法。印製圖案、塗覆或裝飾的薄膜,可含或不含有煙草。印製、塗覆或裝飾的功能之一為增加薄膜的著色劑、調味或煙草之額外量。另一個功能為改善尺寸安定性及薄膜的外觀。一旦製備了印製、塗覆或裝飾的薄膜,可再添加一層特別的薄膜去覆蓋、保護與密封該經印製、塗覆或裝飾的表面。
下表顯示製造本發明之薄膜例示成分:
將DOW化學公司之50g K-3(60%),K-100(35%)與K-4M(5%)
等級之羥丙基甲基纖維素(Hydroxypropylmethyl Cellulose,HPMC)之混合物加入攪拌良好,經加熱至溫度180℉之含有450g去離子水的燒杯內。攪拌下,40g磨細的煙草與15g的微晶纖維素microcrystalline cellulose(FMC),17g澱粉(B-700來自Grain Processing Corp.),16g甘油,0.8g聚山梨醇酯80(polysorbate 80,Unichema),與4g的丙二醇單硬脂酸酯(Propylene Glycol Monostearate,PGMS,Danisco),加入HPMC溶液。當溫度下降低於100℉,加入10g肉桂香料與2g人工甜味料蔗糖素(Sucralose),以2g的碳酸鈉調整pH值至約7.5。當上述成分全部加入且均勻分散後,置入65℉的水浴中持續攪拌30分鐘,加入適量的水使Brookfield黏度在65℉時達5000厘泊(centipoise)。
取部份上述溶液以刮墨測試刮刀(Draw down blade)採定距(fixed gap)15密耳(mils)(0.015英吋)攤平於玻璃板,再將此玻璃板置於170℉空氣循環的實驗室烘箱內。30分鐘後,將玻璃板由烘箱移出,冷卻至室溫,乾燥後約具0.0025英吋厚度之薄膜由玻璃板移出。該薄膜可切成適於入口的的大小。1英吋x 1.25英吋的薄膜段在口腔中崩解的時間點形地少於一分鐘,同時釋出調味與甜味料和煙草的味道。此薄膜中的煙草含量,基於乾重約為25%。
使用與實施例B相同步驟,製備不加入煙草之溶液,當溶液仍熱時,攪拌下加入32g二氧化鈦懸浮液(水中50%二氧化鈦,Sensient Colors公司)與0.01g的FD&C Red 40著色劑(Sensient Colors公司)。溶液冷卻至65℉,如實施例B步驟經攤平於玻璃板,乾燥並由玻璃板移出薄膜。可獲得不透明,淺紅色,高強度的15密耳(mils)(0.015英吋)薄膜。
取部份實施例B溶液,以刮刀(Draw down blade)採定距15密耳攤平於玻璃板。將此玻璃板置於實驗室烘箱內乾燥如實施例B。該玻璃板由烘箱移出且冷卻至室溫,但不由玻璃板移出薄膜。
取部份實施例C溶液以刮刀(Draw down blade)採定距5密耳(0.005英吋)攤平於乾燥後含有實施例B薄膜的玻璃板。將此玻璃板置於170℉實驗室烘箱內10分鐘。由玻璃板移出乾燥後具3密耳(0.003英吋)厚度的薄膜。該薄膜有不同兩側,一邊為含有煙草的棕色薄膜,另一邊為含有香料的紅色薄膜。該薄膜之1英吋x 1.25英吋之小段,在口腔中崩解的時間少於一分鐘。
取部份實施例C溶液以刮刀(Draw down blade)採定距5密耳攤平於玻璃板,且將此玻璃板置於實驗室烘箱內並乾燥如前所述。取部份實施例B溶液以刮刀(Draw down blade)採定距15密耳攤平於含有乾燥後的實施例C薄膜的玻璃板,將此玻璃板置於實驗室烘箱內並乾燥如前所述。取部份實施例C溶液以刮刀(Draw down blade)採定距5密耳攤平於含有乾燥薄膜的玻璃板,並以實驗室烘箱乾燥如前所述。所得薄膜厚度為3密耳且包含三層薄膜,中心為含有煙草的棕色薄膜,兩邊為含有香料的紅色薄膜,薄膜之1英吋x 1.25英吋之小段在口腔中崩解的時間少於一分鐘。
取100g之含煙草之實施例B溶液,於劇烈攪拌時加入0.5g硫酸月桂酸酯鈉(sodium lauryl sulfate;SDS)界面活性劑。之後再以高剪力攪拌機,如型號L4RT-W的Silverson Laboratory Homogenizer均質機,混合成帶有均勻發泡的溶液。此溶液以刮刀(Draw down blade)採定距4密耳攤平於玻璃
板,且於實驗室烘箱內並乾燥。由玻璃板取下後獲得乾燥且厚度為4密耳(0.004英吋)的發泡薄膜,薄膜之1英吋x 1.25英吋之小段,重量約為實施例B中相同大小非發泡薄膜的35%。相較於實施例B所製造之相同未發泡薄膜,發泡薄膜在口中溶解速率一般較快。
以添加40g噴霧乾燥之阿拉伯膠(Gum Arabic,IIC Gums,Inc.)與0.4g的丙二醇單硬脂酸酯(Propylene Glycol Monostearate,PGMS)至含有60g去離子水的燒杯內,劇烈攪拌30分鐘,製成溶液。於10g該溶液中加入0.01g的FD&C Red 40著色劑且以高速攪伴以卻使該著色劑均勻分散。此溶液經覆蓋後靜置24小時以使其中的空氣逸出。取部份該溶液以刮刀(Draw down blade)採定距5密耳(0.005英吋)攤平於玻璃板,再將此玻璃板置於170℉實驗室烘箱內20分鐘直到完全乾燥。當薄膜由玻璃板移出時,其破裂為高光澤、有著色、紅色薄片之許多小片。以其他的FD&C著色劑多次重複此步驟製造出許多不同著色的薄片。亦可添加調味劑與人工甜味劑致該等薄片。
10g由實施例G製備之溶液加入4g磨細的煙草粉末。以與實施例G相同方法,於玻璃板製備,乾燥、冷卻、及移出薄膜。所得薄片為由50%煙草及50%阿拉伯膠所組成,且為深棕色。亦可依所需加入調味劑。可添加例如碳酸氫鈉之材料製薄片以調整酸鹼值。
同實施例B製備薄膜。當薄膜在玻璃板仍濕時,製備經測定量之薄片且均勻的分散於濕薄膜。於實驗室烘箱內乾燥該玻璃板;該薄膜冷卻至室溫後由玻璃板移出薄膜。典型地,實施例B之乾燥薄膜具有乾重1g(含有煙草25%或0.25g)。當此薄膜
分成20等份薄膜(1英吋x 1.25英吋x 2密耳)時,每個小等份重約50毫克(含有煙草25%或12.5mg)。若1g的煙草小薄片(煙草重量百分比為50%)均勻分散於薄膜,則整個薄膜會重2g(煙草總量約0.75g)。當分成20等份時,每個小等份重約100毫克且含煙草37.5毫克。切割為1英吋x 1.25英吋之小段薄膜在口腔中崩解的時間少於一分鐘。
重複實施例I之步驟但加入裝飾性薄片(彩色的小碎薄片但不含煙草)或經著色之小薄片與含煙草之小薄片之混合物。所得薄膜具有彩色外觀。
下列成分經稱重後合併於具合適體積之容器內:
所得混合物混合至均質態。另一容器稱種下列成分:
稱重沸水619.4克於不鏽鋼容器中。水以高剪力混合機Arrow Model 1750劇烈攪拌。水中加入MIX2。繼續攪拌30秒後加入MIX1。繼續劇烈攪拌4分鐘。所得溶液中加入MIX3。劇烈攪拌繼續一分鐘。所得溶液移入適於真空下攪拌之Silverson SS1的容器。將此容器連接於Silverson L4RTU均質機馬達單元。溶液於真空下(20至25英吋汞柱),7500RPM速度攪拌2分鐘,之後均質機容器四周放置冰浴。繼續於真空下以10,000RPM速度均質化8分鐘。完成均質化後,溶液之部份移至500毫升的Nalgene瓶以儲存。
將部份所得凝膠溶液倒在已覆蓋一層適當尺寸之Mylar薄片的玻璃板。以刮刀(draw-down knife)採定距15密耳將膠溶液攤平於玻璃板。將此玻璃板置於75℃送風定溫烘箱(side-swept forced air oven)(VWR model 1330FM)內30分鐘。所得薄膜乾燥到含約4%溼度,由Mylar薄片移出此薄膜並切成適當尺寸單位。薄膜之1英吋x 1.25英吋單位在口腔中崩解的時間少於30秒。
在口腔中崩解的時間相對略長的薄膜(在口腔中崩解的時
間多於30秒之薄膜)可以用刮刀(draw-down knife)採定距30密耳將該溶液鑄型(casting)攤平於玻璃板來獲得。該薄膜以上述相同方式乾燥所需時間為40分鐘。此薄膜在口腔中崩解的時間典型地少於一分鐘。
在口腔中崩解超快的薄膜(在口腔中崩解的時間少於15秒之薄膜)可由相同的溶液於鑄型於該玻璃板之前,藉發泡該溶液而製成。發泡係將各100g溶液,進行高剪力混合(高剪力混合機Arrow Model 1750)約3分鐘,再隨即用刮刀(draw-down knife)採定距30密耳鑄型於玻璃板上來獲得。此種薄膜在口腔中崩解的時間典型地少於15秒。
下列成分經稱重後合併於具合適體積之容器內:
所得混合物混合至均質態。另一容器稱種下列成分:
混合物2(MIX2)
稱重沸水619.4克於不鏽鋼容器中。水以高剪力混合機Arrow Model 1750劇烈攪拌。水中加入MIX2。繼續攪拌30秒後加入MIX1。繼續劇烈攪拌4分鐘。所得溶液中加入MIX3。劇烈攪拌繼續一分鐘。所得溶液移入適於真空下攪拌之Silverson SS1的容器。將此容器連接於Silverson L4RTU均質機馬達單元。溶液於真空下(20至25英吋汞柱),7500RPM速度攪拌2分鐘,之後均質機容器四周放置冰浴。繼續於真空下以10,000RPM速度均質化8分鐘。完成均質化後,溶液之部份移至500毫升的Nalgene瓶以儲存。
將部份所得凝膠溶液倒在已覆蓋一層適當尺寸之Mylar薄片的玻璃板。以刮刀(draw-down knife)採定距15密耳將膠溶液攤平於玻璃板。將此玻璃板置於75℃送風定溫烘箱(side-swept forced air oven)(VWR model 1330FM)內30分鐘。所得薄膜乾燥到含約4%溼度,由Mylar薄片移出此薄膜並切成適當尺寸單位。薄膜之1英吋x 1.25英吋單位在口腔中崩解的時間典型地為15至30秒。
或者,此薄片調味劑可包含冬青,綠薄荷或蘋果。
在口腔中崩解的時間相對略長的薄膜(在口腔中崩解的時
間多於30秒之薄膜)或崩解超快的薄膜(在口腔中崩解的時間少於15秒之薄膜)可由如同實施例K的溶液製得。
下列成分經稱重後合併於具合適體積之容器內:
所得混合物混合至均質態。另一容器稱種下列成分:
稱重沸水619.4克於不鏽鋼容器中。水以高剪力混合機Arrow Model 1750劇烈攪拌。水中加入MIX2。繼續攪拌30秒後加入MIX1。繼續劇烈攪拌4分鐘。所得溶液中加入MIX3。劇烈攪拌繼續一分鐘。所得溶液移入適於真空下攪拌之Silverson SS1的容器。將此容器連接於Silverson L4RTU均質機馬達單元。溶液於真空下(20至25英吋汞柱),7500RPM速度攪拌2分鐘,之後均質機容器四周放置冰浴。繼續於真空下(20至25英吋汞柱)以10,000RPM速度均質化8分鐘。完成均質化後,溶液之部份移至500毫升的Nalgene瓶以儲存。
將部份所得凝膠溶液倒在已覆蓋一層適當尺寸之Mylar薄片的玻璃板。以刮刀(draw-down knife)採定距15密耳將膠溶液攤平於玻璃板。將此玻璃板置於75℃送風定溫烘箱(side-swept forced air oven)(VWR model 1330FM)內30分鐘。所得薄膜乾燥到含約4%溼度,由Mylar薄片移出此薄膜並切成適當尺寸單位。薄膜之1英吋x 1.25英吋單位在口腔中崩解的時間典型地為15至30秒。
在口腔中崩解的時間相對略長的薄膜(在口腔中崩解的時間多於30秒之薄膜)或崩解超快的薄膜(在口腔中崩解的時間少於15秒之薄膜)可由如同實施例K的溶液製得。
表N1
下列成分經稱重後合併於具合適體積之容器內:
所得混合物混合至均質態。另一容器稱種下列成分:
稱重沸水606.10克於不鏽鋼容器中。水以高剪力混合機
Arrow Model 1750劇烈攪拌。水中加入MIX2。繼續攪拌30秒後加入MIX1。繼續劇烈攪拌4分鐘。所得溶液中加入MIX3。劇烈攪拌繼續一分鐘。所得溶液移入適於真空下攪拌之Silverson SS1的容器。將此容器連接於Silverson L4RTU均質機馬達單元。溶液於真空下(20至25英吋汞柱),7500RPM速度攪拌2分鐘,之後均質機容器四周放置冰浴。繼續於真空下(20至25英吋汞柱)以10,000RPM速度均質化8分鐘。完成均質化後,溶液之部份移至500毫升的Nalgene瓶以儲存。
將部份所得凝膠溶液倒在已覆蓋一層適當尺寸之Mylar薄片的玻璃板。以刮刀(draw-down knife)採定距20密耳將膠溶液攤平於玻璃板。將此玻璃板置於75℃送風定溫烘箱(side-swept forced air oven)(VWR model 1330FM)內35分鐘。所得薄膜乾燥到含約4%溼度,由Mylar薄片移出此薄膜並儲存於塑膠袋中供將來使用。
或者經調味之煙草薄膜,例如經蘋果調味,由後述配方及步驟製備。
下列成分經稱重後合併於具合適體積之容器內:
所得混合物混合至均質態。另一容器稱種下列成分:
稱重沸水606.10克於不鏽鋼容器中。水以高剪力混合機Arrow Model 1750劇烈攪拌。水中加入MIX2。繼續攪拌30秒後加入MIX1。繼續劇烈攪拌4分鐘。所得溶液中加入MIX3。劇烈攪拌繼續一分鐘。所得溶液移入適於真空下攪拌之Silverson SS1的容器。將此容器連接於Silverson L4RTU均質機馬達單元。溶液於真空下(20至25英吋汞柱),7500RPM速度攪拌2分鐘,之後均質機容器四周放置冰浴。繼續於真空下(20至25英
吋汞柱)以10,000RPM速度均質化8分鐘。完成均質化後,溶液之部份移至500毫升的Nalgene瓶以儲存。
將部份所得凝膠溶液倒在已覆蓋一層適當尺寸之Mylar薄片的玻璃板。以刮刀(draw-down knife)採定距20密耳將膠溶液攤平於玻璃板。將此玻璃板置於75℃送風定溫烘箱(side-swept forced air oven)(VWR model 1330FM)內35分鐘。另外的薄膜鑄型於40密耳且乾燥1小時。所得薄膜乾燥到含約4%溼度,由Mylar薄片移出此薄膜並儲存於塑膠袋中供將來使用。
替代的調味如薄菏味、冬青味或綠薄菏味。替代的著色包括FD & C藍色Alum Lake 35-42%、FD & C翡翠綠Lake Blend、與FD & C藍色Alum Lake加上FD & C翡翠綠Lake Blend。
下列成分經稱重後合併於具合適體積之容器內:
所得混合物混合至均質態。另一容器稱種下列成分:
稱重沸水606.10克於不鏽鋼容器中。水以高剪力混合機Arrow Model 1750劇烈攪拌。水中加入MIX2。繼續攪拌30秒後加入MIX1。繼續劇烈攪拌4分鐘。所得溶液中加入MIX3。劇烈攪拌繼續一分鐘。所得溶液移入適於真空下攪拌之Silverson SS1的容器。將此容器連接於Silverson L4RTU均質機馬達單元。溶液於真空下(20至25英吋汞柱),7500RPM速度攪拌2分鐘,之後均質機容器四周放置冰浴。繼續於真空下(20至25英吋汞柱)以10,000RPM速度均質化8分鐘。完成均質化後,溶液之部份移至500毫升的Nalgene瓶以儲存。
將部份所得凝膠溶液倒在已覆蓋一層適當尺寸之Mylar薄片的玻璃板。以刮刀(draw-down knife)採定距20密耳將膠溶液攤平於玻璃板。將此玻璃板置於75℃送風定溫烘箱
(side-swept forced air oven)(VWR model 1330FM)內35分鐘。所得薄膜乾燥到含約4%溼度,由Mylar薄片移出此薄膜並儲存於塑膠袋中供將來使用。
下列成分經稱重後合併於具合適體積之容器內:
所得混合物混合至均質態。另一容器稱種下列成分:
稱重沸水606.10克於不鏽鋼容器中。水以高剪力混合機Arrow Model 1750劇烈攪拌。水中加入MIX2。繼續攪拌30秒後加入MIX1。繼續劇烈攪拌4分鐘。所得溶液中加入MIX3。劇烈攪拌繼續一分鐘。所得溶液移入適於真空下攪拌之Silverson SS1的容器。將此容器連接於Silverson L4RTU均質機馬達單元。溶液於真空下(20至25英吋汞柱),7500RPM速度攪拌2分鐘,之後均質機容器四周放置冰浴。繼續於真空下(20至25英吋汞柱)以10,000RPM速度均質化8分鐘。完成均質化後,溶液之部份移至500毫升的Nalgene瓶以儲存。
將部份所得凝膠溶液倒在已覆蓋一層適當尺寸之Mylar薄片的玻璃板。以刮刀(draw-down knife)採定距20密耳將膠溶液攤平於玻璃板。將此玻璃板置於75℃送風定溫烘箱(side-swept forced air oven)(VWR model 1330FM)內35分鐘。所得薄膜乾燥到含約4%溼度,由Mylar薄片移出此薄膜並儲存於塑膠袋中供將來使用。
下列成分以本文所述類似用於錠劑製造之造粒(granulations)方式造粒,獲得溼度4.50%的煙草顆粒:
將煙草顆粒置入雙螺桿擠出機(Leistritz Micro-18 Twin Screw Extruder 40:1 L/D)的饋料口,此饋料口經配置於中度剪力螺桿設計共同旋轉擠出裝置。擠出之饋料速度自每小時1至3磅不等。汽缸區溫度自75至240℉不等。擠出成形的通風揮發藉著擠出機排放模具(discharge die)前加入通風孔而達成。
寬約3英吋厚約2至3密耳的煙草薄膜乃藉著在擠出機排放端加入料條模具(strip die)而成。排放時煙草薄膜藉著3個滾輪架起的冷卻滾筒輪壓及冷卻至室溫。薄膜在冷卻滾筒的後方由捲輪迴轉,加上Mylar層於薄膜之間以避免相黏。該煙草薄膜置入適於儲存之容器。
如本文所述,該煙草薄膜用於製造含袋狀之可溶解煙草。該薄膜在口中會崩解緩慢,經2至4分鐘期間。
下列成分經稱重後合併於具合適體積之容器內:
所得混合物混合至均質態。另一容器稱種下列成分:
稱重沸水288.93克於不鏽鋼容器。以高剪力混合機Arrow Model 1750劇烈攪拌。水中加入MIX2,繼續攪拌30秒後加入MIX1。繼續劇烈攪拌4分鐘。所得溶液中加入MIX3。繼續劇烈攪拌3分鐘。所得溶液移入適於儲存的容器。
將部份所得凝膠溶液倒在已覆蓋一層適當尺寸之Mylar薄
片的玻璃板。以刮刀(draw-down knife)採定距20密耳將膠溶液攤平於玻璃板。將此玻璃板置於75℃送風定溫烘箱(side-swept forced air oven)(VWR model 1330FM)內35分鐘。所得薄膜乾燥到含約4%溼度,由Mylar薄片移出此薄膜並切成適當尺寸單位。薄膜之1英吋x 1.25英吋單位在口腔中崩解的時間少於30秒,釋放出調味、甜味與煙草。
下列成分經稱重後合併於具合適體積之容器內:
所得混合物混合至均質態。另一容器稱種下列成分:
以第三容器稱重下列成分:
稱重沸水288.93克於不鏽鋼容器。以高剪力混合機Arrow Model 1750劇烈攪拌。水中加入MIX2,繼續攪拌30秒後加入MIX1。繼續劇烈攪拌4分鐘。所得溶液中加入MIX3。繼續劇烈攪拌3分鐘。所得溶液移入適於儲存的容器。
將部份所得凝膠溶液倒在已覆蓋一層適當尺寸之Mylar薄片的玻璃板。以刮刀(draw-down knife)採定距20密耳將膠溶液攤平於玻璃板。將此玻璃板置於75℃送風定溫烘箱(side-swept forced air oven)(VWR model 1330FM)內35分鐘。所得薄膜乾燥到含約4%溼度,由Mylar薄片移出此薄膜並切成適當尺寸單位。薄膜之1英吋x 1.25英吋單位在口腔中崩解的時間少於30秒,釋放出調味、甜味與煙草。
下列成分經稱重後合併於具合適體積之容器內:
所得混合物混合至均質態。另一容器稱種下列成分:
稱重沸水288.93克於不鏽鋼容器。以高剪力混合機Arrow Model 1750劇烈攪拌。水中加入MIX2,繼續攪拌30秒後加入MIX1。繼續劇烈攪拌4分鐘。所得溶液中加入MIX3。繼續劇烈攪拌3分鐘。所得溶液移入適於儲存的容器。
將部份所得凝膠溶液倒在已覆蓋一層適當尺寸之Mylar薄
片的玻璃板。以刮刀(draw-down knife)採定距20密耳將膠溶液攤平於玻璃板。將此玻璃板置於75℃送風定溫烘箱(side-swept forced air oven)(VWR model 1330FM)內35分鐘。所得薄膜乾燥到含約4%溼度,由Mylar薄片移出此薄膜並切成適當尺寸單位。薄膜之1英吋x 1.25英吋單位在口腔中崩解的時間少於30秒,釋放出調味、甜味與煙草。
本發明之組合物亦可製成錠劑,如超快速崩解錠(約15秒)、快速崩解錠(少於2分鐘)、慢速崩解錠(2至10分鐘)及口嚼錠。
錠劑在口中之大小可以為個人使用量或更小,以多重錠劑組成個人用量。按個人用量製作之組合物的錠劑典型地為5mm至15mm的長度。小的錠劑典型地直徑範圍為2至4mm。該等小的錠劑可以製造成不同種類的著色劑或調味劑,如供同時使用。錠劑會以薄片、凸圓或凹球狀丸形、卵形或任一其他的已知形狀販售。錠劑也可以發泡製造以提供快速在口中溶解或崩解。錠劑也可以多層的方式製造,當錠劑溶解或崩解時,提供不同種類的味道或口感。錠劑亦可加上塗覆以修改著色或味道,或者提供機械張力以便於取用。在一具體例中,經設計成在水中快速崩解的錠劑會經以非常薄的不溶性塗覆包裹以保護錠劑的第二層水溶型塗覆。
錠劑可以由乾性混合物來製造,如已知的直接壓縮法,或由預顆粒化材料經任一已知技術上的錠劑方法製造,如經壓縮、注入成形、加壓成形、發泡注入成形或發泡加壓成形。
下表顯示用於製造本發明之錠劑之例示成分:
咀嚼錠可以經由下列成分製造:濃縮糖(40%),煙草(20%),葡萄糖(25%),麥芽糊精(13%),著色劑(0.05%),調味劑(1.35%),與硬脂酸酯鎂(0.60%)。
熱塑性錠劑可以經由下列成分製造(以份量計):羥丙基纖維素(Hydroxypropyl Cellulose,HPC)54,煙草27,微結晶纖維素10,丙二醇10,人工甜味劑2,調味劑2,安定劑0.2。該等成分在乾燥時混合,饋料於汽缸溫度設定於可融解HPC之溫度(一般為340至370℉)的擠出機。擠壓出約1/2英吋之柱狀體,再切成足以形成錠劑的大小。
表AB2 用於製造煙草錠劑之結合液配方
稱重數量如表AB2所示之成分於不同的容器中。預水合之阿拉伯膠(gum arabic pre-hydrated)(乳化劑)緩慢加入水中並在不鏽鋼容器中以高剪力攪動。當完全溶解後緩慢將M585麥芽糊精(Grain Processing Corporation)加入水中。一旦M585完全溶解,緩慢加入甜味劑蔗糖素溶液(Tate & Lyle),且攪拌均勻以確保完全溶解。
如表AB1之薄菏與綠薄菏調味劑和碳酸鈉之配方量加入該結合液。整體混合物以均質機9000至10000RPM轉速,均質化20分鐘。結合液之數量依批次大小與表AB所示之成分百分比而定。均質化之溶液轉移至調味劑儲存/抽送槽中。
將甘露醇(甜味劑)與煙草粉末依表AB1之配方量混合並置放於產品缽中。
最終造粒過程採用Vector Multiflo-15流化床包衣機將結合液與混勻的乾燥成分共同配製。自電腦控制面板選取手動程式。機械操作參數係,表AB3所列出者,載至程式:
用來噴灑的結合液之適宜量亦載於程式中。依所需的批次大小由表AB1中顯示的成分百分比決定結合液之份量。
一旦乾燥成分在流體床腔內流動且溫度達到40至45℃後,使結合液緩慢的噴灑於乾燥成分以形成顆粒化。噴嘴的壓力設定於22psi,風量達200CFM。風量增加到足以使流體床腔內產品移動或流動程度。結合液全噴灑完後再降低風量至200CFM。當產品溫度為約43℃時此步驟即停止。
顆粒化材料以12-網眼過篩。硬脂酸酯鎂(潤滑劑)亦以40-網眼過篩。將硬脂酸酯鎂配方量如表AB4所示與顆粒化材料混於塑膠袋中,手工搖動約2分鐘。
顆粒化材料加上潤滑劑置於擠壓機的投入口,表AB5列出Vanguard VSP 8 Mini Rotary Press擠壓機操作的參數:
快速崩解:在口腔中崩解的時間1至3分鐘
慢速崩解:在口腔中崩解的時間5至8分鐘
結合液之製備步驟依據實施例AB1之結合液之製備。薄荷與綠薄荷造粒程序的配方量,如表AC1所示,並加入45g碳酸鈉於結合液中。除了補充結合液外其餘的步驟如乾燥成分之製備、Vector Multiflo-15流體床腔之制備及造粒程序均如前所述。
顆粒化材料加上潤滑劑硬脂酸酯鎂經前述同樣的程序篩選大小,將硬脂酸酯鎂之配方量(快速崩解:0.75%;慢速崩解:1.00%)與顆粒化的材料混於塑膠袋中,手工搖動約2分鐘。
表AC3列出Vanguard VSP 8 Mini Rotary Press擠壓機操作的參數:
結合液之製備步驟同前述之製備方式。肉桂調味劑與碳酸鈉的配方量,如表AD1所示加入於結合液中。其餘的步驟如補充結合液、乾燥成分之製備(乳糖填充劑與煙草粉末)、Vector Multiflo-15流體床腔之製備及造粒程序均如前所述。
顆粒化材料加上潤滑劑硬脂酸酯鎂各經12-網眼與40-網眼篩選大小,將硬脂酸酯鎂之配方量(快速崩解:0.50%;慢速崩解:1.00%)與顆粒化的材料混於塑膠袋中,手工搖動約2分鐘。
列於表AD3之參數經設定於Vanguard VSP 8 Mini Rotary Press擠壓機:表AD3.用於煙草錠劑之定形物形成參數
煙草錠劑之製備步驟同實施例AD之製備方式,惟以冬青調味劑取代肉桂調味劑。
上述完成之材料經12-網眼過篩,潤滑劑硬脂酸酯鎂經40-網眼篩選大小,將硬脂酸酯鎂之配方量(快速崩解:0.50%;慢速崩解:0.75%)與顆粒化的材料混於塑膠袋中,手工搖動約2分鐘。
列於表AE1之參數經設定於Vanguard VSP 8 Mini Rotary Press擠壓機:
結合液之製備步驟同前述之製備方式。蘋果調味劑、天然抑苦劑(Comax)與碳酸鈉的配方量,如表AF1所示加入於結合液中。其餘的步驟如補充結合液、乾燥成分之製備(乳糖填充劑與煙草粉末)、Vector Multiflo-15流體床腔之製備及造粒程序均如前所述。
上述完成之材料經12-網眼過篩,潤滑劑硬脂酸酯鎂經40-
網眼篩選大小,將硬脂酸酯鎂之配方量(慢速崩解:0.75%)與
顆粒化的材料混於塑膠袋中,手工搖動約2分鐘。
列於表AF3之參數經設定於列出Vanguard VSP 8 Mini Rotary Press擠壓機:
依製造商的說明配置20% Opadry II膜衣液,並在塗覆處
理前混合45分鐘。
將錠劑(5.5至6.5KG)置於塗料器(Vector/Freund Hi-Coater pan coating machine)的塗覆鍋中(Coating pan)且加熱直到排氣溫度達45℃。塗覆鍋轉速需小於5RPM以避免錠劑的摩擦。空氣以溫度75℃和風量100CFM通過該鍋子達到-0.5英吋水壓力。
當錠劑到達溫度時,塗覆鍋轉速增為約15RPM,以15置20g/min的速率施用Opadry塗覆液。施用期間持續攪拌懸浮液以避免形成固體。以約每分鐘100L空氣近70psi的高壓噴灑。高壓噴灑的形式以噴嘴的定向空氣通口設定約每分鐘50L空氣近70psi。
入口氣體溫度週期性的增或減以維持排氣溫度界於43至46℃。
噴灑工作持續進行直至所需固體量施用至滿足配方所需量,一般為約3%,或至錠劑為視覺性滿足。
下列成分稱重於各自容器:
加水6g於碳酸鈉,並攪拌混合物。持續攪拌此混合物直到此步驟稍後將其加至其他成分。
水部分2(冷)置於冰浴中冷卻,而水部分1(熱)加熱至60℃且移至不鏽鋼容器。該60℃水以高剪力混合機Arrow Model 1750劇烈攪拌,逐漸加入Klucel EF。此溶液繼續攪拌數分鐘。之後水部分2(冷)加至混合物。冰浴置於不鏽鋼容器下,且繼續攪拌此混合物15分鐘。
攪拌15分鐘後,加入其餘成分製混合物,一次一項。加入次一成分前完全攪拌混合物。成分添加次序:煙草調味改質劑、丙二醇、蔗糖素溶液、玉米糖漿、碳酸鈉溶液、蔗糖、煙草粉末、B700及薄荷油。混合步驟中持續加入冰塊至冰浴以保持混合物冷卻。所有成分添加後,此混合物另劇烈攪拌10分鐘。
自冰浴取出容器,將混合物倒在蠟紙上分散成可崩解固體部分並於室溫乾燥24小時。由蠟紙上移出可崩解固體再放至另一張蠟紙上繼續於室溫乾燥。可崩解固體所需之硬度在12至24小時持續乾燥後達成。
下列成分稱重於各自容器:
加水6g於碳酸鈉,並攪拌混合物。持續攪拌此混合物直到此步驟稍後將其加至其他成分。
水部分1(熱)加熱至80℃且移至不鏽鋼容器。該80℃水以高剪力混合機Arrow Model 1750劇烈攪拌,逐漸加入HPMC。此溶液繼續攪拌數分鐘。之後水部分2(室溫)加至混合物,且繼續攪拌此混合物15分鐘。
攪拌15分鐘後,加入其餘成分製混合物,一次一項。加入次一成分前完全攪拌混合物。成分添加次序:煙草調味改質劑、丙二醇、蔗糖素溶液、玉米糖漿、碳酸鈉溶液、蔗糖、煙草粉末、B700及薄荷油。所有成分添加後,此混合物另劇烈攪拌10分鐘。
自冰浴取出容器,將混合物倒在蠟紙上分散成可崩解固體部分並於室溫乾燥24小時。由蠟紙上移出可崩解固體再放至另一張蠟紙上繼續於室溫乾燥。可崩解固體所需之硬度在12至24小時持續乾燥後達成。
類似的產品依相同的配方,混合步驟及分散步驟,但可崩解固體置於32℃送風定溫烘箱(VWR model 1330FM)內乾燥一小時。由烘箱內取出可崩解固體再於室溫下乾燥24小時。此外,也可放置在32℃烘箱內18小時。這樣的乾燥方式獲得略硬之可崩解固體的淡色煙草。
市售可得之加壓設備可用來製備雙層或多層錠劑。組合物
中,該等層的組合物可以相同或不同。各層可依著色、調味、煙草種類、含量、崩解速率與其他類似的特性而不同。例如,單層可快速崩解以釋出調味或調味遮蔽劑。含有煙草的第二層可以慢速的崩解逐漸釋出煙草。
煙草組合物亦可形成足夠堅硬、易於處理的產品。這些成形產品之物理特性可能相異,且其範圍可由高撓性到高硬度不建。該等產品亦可形成任何形狀,並可為緻密性或發泡性。該等組合物通常含有最終產物重量比之2至50%的溼度,較佳為5至10%。例示形狀包含管狀、牙籤狀、棍狀、螺旋狀與細棒狀。典型地,成形部件可供吸食或咀嚼一段較長的時間以於口腔中釋出煙草感官察覺成分。成形部件可為或可不為口中可崩解者。部件可在1至60分鐘期間內崩解,較佳為1至10分鐘。
成形部件的大小可為或可不為適合整個口腔。大於口腔的組合物可只插入部分。一般而言,最大的尺寸為6英吋,較佳為2.5英吋。
成形部件可含有不連續的區塊,例如,每個區塊具有相同或相異的調味、著色、大小、或煙草形式(例如可溶性的煙草)。舉例而言,螺旋體中的雙股(細條)具有相異的調味、著色、大小、或煙草形式。進一步的實施例顯示,成形部件可由多步驟製備,其中鑄形或突起的部件由層所組成,兩層或以上的層其具有相異的調味、著色、大小、或煙草形式。
成形部件組合物可由任何已知技術製造,如擠壓成形,壓縮成形,射出成形,衝擊成形,發泡成形,吹袋成形與注塑成形。此外,成形部件可為水溶性或熱塑性為主之配方。於一具體例中,水相的成形部件由配方、水、煙草、和其他成分形成的黏性糊狀物(例如,經由Hobart擠壓),且擠壓至成形、經鑄模壓出,或形成平板形式再切割成所需形狀而製造。該等切割
或成形的部件可乾燥至2至50%的溼度,堅硬部件溼度較佳為完工後產品重量之5至10%,高撓性部件溼度則為10至50%。在另一具體例中,水相糊狀物可經由雙螺桿擠壓機(Wenger twin screw extruder)在二階段擠壓法(two stage extrusion process)形成,其中該等配方、水、煙草、和其他成分於混合或機器的擠壓前階段混合,所形成的糊狀物直接饋料到擠壓機的雙螺桿擠壓單元,經鑄模擠壓製造成所需形狀,之後乾燥至所需的溼度。熱塑成形部件係,藉由PK混合機、高強力攪拌機、預結粒機或顆粒化步驟(流體床或Hobart)混合成分而製造。經混合的成分可藉著傳統的單或雙螺桿擠壓機來形成成形部件,或者將混合物饋料於射出成形機或其他熱塑成形機以製成成形部件。
下列表提供由射出成形模具形成例示之成形部件:
加熱區溫度範圍設定如後:1區-300至340℉,2區-350至370℉,3區-350至370℉,模具溫度-室溫。加足以達到一次射出成形循環的組合物,饋料於螺桿;這些材料隨即射出到模具上;模具在10秒後打開;且可移出部件。此成形部件為梯狀彩色碎片,2英吋x 3英吋,梯長為1/8、1/4、及3/8吋厚。
下列表提供由壓縮成形模具形成例示之成形部件:
取10至50g水加於100g乾燥成分-足使混合物軟化並使之穿過混合機上的糊狀鑄膜。模具參數如下:
越長的滯留時間製造出越堅固的部件,只要使蒸氣在展延部件時自由通風。也可加入添加劑使成形部件在移出工具時保持可撓性。該等部件含有大量低黏度HPC,如留在工具中較長時間(40至60秒)可形成優良的部份。加入增速劑可增加自空氣中吸收濕度的速度,經過一段時間後會造成一些部件軟化。
當模具孔完全填滿成形材料時,可製備緊密的和堅硬的部件。當模具孔只填滿75%時,該等化合物經過展開蒸氣形成具有良好硬度,調味與在口中逐漸崩解的發泡物件。
水相系統的發泡形式可藉由加入界面活性劑(硫酸月桂酯
鈉)於混合物中再以攪拌器及打使氣泡進入製成;發泡或曝氣程序也可藉著於水相系統中在高剪刀下加入氣體(如氮氣)。水相系統在經由乾燥至所需溼度以製備安定的發泡組合物。在一具體例中,以水性組合物填滿部份壓縮模具;關上模具;加溫超過水的沸點以製造蒸氣,擴展該水性組合物以填入於空隙處,以製造出具有發泡的成形部件。在熱塑系統中,發泡的形成乃藉著加水於煙草/配方組合物;加溫超過水的沸點以製造蒸氣,而後在煙草組合物由鑄模射出時,蒸氣擴展以製造發泡結構。另一具體例中,在熔化熱塑的煙草組合物由擠壓機排出錢先加入氣體(如氮氣或二氧化碳),以便在成形的煙草組合物中造成高度均勻的發泡結構。其他已知的熱塑發泡程序(如射出發泡成形)可用以製造具有發泡的煙草組合物和成形部件。
表AL1和AL2列出本發明製造水相成形部件的例示成分。要加入足量的水以形成有黏性的糊狀物。
表AM1顯示本發明製造熱塑成形部件的例示成分,
煙草桿由煙草(54份)、調味料(2份)、不可溶纖維(28份)、羧甲基纖維素(CMC)(10份)、人工甜味料(0.2份)、微結晶纖維素(30份)所組成。加入足量的水(如140份)以形成有黏性的糊狀物,且該糊狀物適宜經由擠壓機排出。適宜的擠壓機應為裝置有糊狀物排出口和鑄模的廚房用攪拌機(Kitchen Aid mixer)。經由擠壓機糊狀物鑄模製成的煙草桿可用來作為螺旋盤繞機的軸胎,可用含煙草薄膜包裝此煙草核心。
下列成分稱重後一起加入適合的容器:
所得混合物混合至均質態。另一容器稱種下列成分:
MIX1以廚房用立式攪拌機混合於不鏽鋼容器。逐漸加入MIX2,於加上槳葉之攪拌機中慢速攪拌3分鐘以上。接著加入76.92g水,以同樣方式攪拌。所得糊狀物置於室溫下5分鐘。
靜置期間後,將該糊狀物倒入附接於攪拌機上的1/8英吋孔洞細條形成單元。所製成的線形物切割成界於1.5至2英吋長,並存放在適合容器內。
將一組正對著洞口2x1/4英吋的壓印板加熱至300至330℉。所形成的長條置於下方孔洞,且模具藉著水壓關閉。模具關閉期間為30至60秒,藉著這個方法煮熟產品內的澱粉成分並釋出部份揮發性材料。
新製成的煙草棒,約為2x1/8英吋的大小含有堅硬的外層與堅硬的類似發泡內層。此單元產品在口腔中崩解的時間為1至2分鐘。
下列成分經稱重後合併於具合適體積之容器內:
上述混合物混至均質態。另以容器稱重下列成分:
MIX1以廚房用立式攪拌機混合於一不鏽鋼容器。逐漸加入MIX2,於加上槳葉之攪拌機中慢速攪拌3分鐘以上。接著加入76.95g水,以同樣方式攪拌,置於室溫下5分鐘。
靜置期間後,將該糊狀物倒入附接於攪拌機上的1/8英吋孔洞細條形成單元。所製成的線形物切割成界於1.5至2英吋長,並存放在適合容器內。
將一組正對著洞口2x1/4英吋的壓印板加熱至300至330℉。所形成的長條置於下方孔洞,且模具藉著水壓關閉。模具關閉期間為30至60秒,藉著這個方法煮熟產品內的澱粉與糖類成分並釋出部份揮發性材料。
新製成的煙草棒,約為2x1/8英吋的大小含有堅硬的外層與堅硬的類似發泡內層。此單元產品在口腔中崩解的時間為1至2分鐘。
下列成分顆粒化過程與錠劑製程相同,製造出濕度約為4.5%的煙草顆粒:
將煙草顆粒置入18mm雙螺桿擠出機(Leistritz Micro-18 Twin Screw Extruder 40:1 L/D)的饋料口,此饋料口經配置與中剪力螺桿設計共同旋轉擠出裝置。饋料速度變化於每小時1至3磅。汽缸區溫度變化於75至100℉。調味劑加入速率為製程流速的5%;於是肉桂調味劑的加入在顆粒饋料的下游。擠出成形的通風揮發藉著擠出機排放模具前加入通風孔而達成。
直徑約1/8英吋的煙草棒乃藉著在擠出機排放端加入線性鑄模而成。排放時柔軟的煙草棒藉著氣冷式輸送帶冷卻至室溫
並變硬,及煙草棒切割成2.5英吋的長度。所形成煙草棒再置入適於儲存之容器。該煙草棒在口中會慢慢溶解,約需5至10分鐘期間。
本發明之組合物亦可製成凝膠或凝膠粒。組合物可含帶有煙草的可溶性或不可溶性凝膠。凝膠可以用來包埋另一材料,或者另一材料可用來包埋凝膠。凝膠的水分含量可高達70%,乾燥後的產品含水量可達1至70%,凝膠中所含的水量取決於經完成產品所需的特性。含有煙草之凝膠製備可提供範圍相當廣泛的感官察覺特性。
可溶性或不可溶性凝膠的配方實施例包括卡帕角叉菜膠、海藻膠鈉、羧甲基纖維素、明膠、果膠、洋菜、與澱粉。
含有煙草之可溶性凝膠可藉著提高溫度溶解配方,如卡帕角叉菜膠在180℃,劇烈攪拌時加入煙草粉末至此溶液。接著將熱溶液倒入模型內。室溫下明膠提供較軟凝膠,其硬度與安定度可藉著增加洋菜或澱粉來完成。其他膠狀劑形可以類似方式製造。
不可溶性凝膠係藉著在事先溶解的溶液或漿狀物中加入交聯劑而形成。將該溶液倒入模型內製成所需形狀,且以冷卻或乾燥的方式定型。多數的例子中要保持高溫,例如高於180℉,以避免在進入模型前過早的凝結。當凝膠製成最終形狀後,可直接以現況包裝或再進一步乾燥至所需水分。交聯劑包括角叉菜膠的鉀離子,海藻膠鈉和低甲氧基果膠的鈣離子,以及羧甲基纖維素的三價離子如鋁離子。不可溶性凝膠(不會在口腔中崩解的)之煙草感官材料在含著或是咀嚼時可能會由凝膠中過濾出來。
一具體例中,凝膠組合物,如粒狀物,具有固態或液態的中心。例示的固態中心包括無煙煙草。內部液體可為水相,非
水相或混合相,取決於包裹粒狀物壁的溶解性。水相液體通常包裹在不可溶性凝膠中,在口中可以經由機械性或化學性的方式破壞。包裹凝膠粒配方可包括聚合物和交聯劑,例示的系統包括角叉菜膠與單價離子(如鉀離子);海藻膠鈉或低甲氧基果膠和二價離子(如鈣離子);以及羧甲基纖維素和三價離子如鋁離子;及明膠和阿拉伯樹脂。其中心可包含或不包含煙草。
另一具體例中,水可溶凝膠包裹非水相填充物,例如施用的乙醇、甘油、蔬菜油、或礦物油。水可溶凝膠與/或非水相填充物可含有煙草或本發明之其他成分。水相液體亦可包埋加入添加物如足以結合填充在內的水的糖或鹽的水相液體,如此避免液體中的水溶解包裝物。凝膠包裝物亦包括標準的硬和軟的明膠膠囊,內部可以固體或液體填充。
凝膠組合物中心可包括或不包括煙草,如煙草漿狀物。凝膠包裝物亦可包括或不包括煙草。例示的固態中心包括無煙煙草。該中心亦可包括著色劑、甜味劑,調味劑或者調味遮蔽劑,可與寧交包裝物相似或相異。凝膠包裝物與中心的崩解速率亦可相同或相異。含有中心的凝膠一般較大,最大可達10mm,如最大5mm。含有液體中心的凝膠粒可經由加入煙草/配方之混合物的微滴於造成凝膠粒外表面凝化的溶液中並留存於液體中心。凝膠粒可以Morishita Jintan公司及其他公司之商業製程”無縫液體包埋(seamless liquid encapsulation)”或”無縫膠囊(seamless capsule)”技術來製造。另外還有普遍使用,由海藻膠鈉、角叉菜膠或果膠聚合物之供應商所發展的製造凝膠的各類方法。藉著改變配方的濃度,交聯劑(如鹽類)的濃度,固化溶液的溫度,與凝膠粒在固化液中的滯留時間,可控制凝膠化的量,因此可控制凝膠包裝物的厚度。該溶液可包括交聯劑或以其他方法誘使凝膠化,如溫度的改變。
固態凝膠可為可溶性或不可溶性。固態凝膠一般係將煙草
和配方,添加物的加入與否,混合而成,配方亦可膠化。可溶性凝膠可以採用自凝樹脂,例如結冷膠(gellan gum)或卡帕角叉菜膠;或採用經由溫度變化固定的聚合物,如明膠而製造。不可溶性凝膠使用交聯劑製備。該等可溶性或不可溶性凝膠可經由加入微滴在如玉米油的油浴中或是水性、含交聯劑溶液浴中來生產球型小滴。亦可使用穿越油浴到達水性交聯劑溶液的方式製造。凝膠亦可在模具中或由鑄膜切割薄片來製造。
另一具體例中,凝膠組合物以配方、交聯劑(如鹽類)、煙草(如粉末狀)的乾燥混合物如粉末型式提供,使用前再由消費者溶合。溶合作用造成凝膠組合物固化,可以直接放入口中。一般而言,消費者將乾燥混合物放在模具中再加入水性或非水性的溶劑,混合物快速的吸水,凝膠形成模具的形狀。所加入的溶劑可添加調味或組合物中的其他風味口感。或者,消費者可直接將乾燥混合物放入口中溶化。溶劑可給予組合物調味或著色。
100g 4%羧甲基纖維素CMC-7MF溶液和20g煙草混合。滴入水可溶,可食的三價鹽(如氯化鋁或硫酸鋁)之5%溶液。微滴的表面以空氣乾燥或烘箱微乾。
100g之2%卡帕角叉菜膠和煙草混合並加熱至180至190℃,滴入冷的5%氯化鉀溶液。
100g之4%中黏度海藻膠鈉溶液和煙草混合並加熱至150至170℉,滴入5%可食的二價鹽(如氯化鈣)之冷溶液。
帶有明膠壁與煙草漿狀物中心的煙草粒可藉著將冷的煙草漿狀物(如60℉)滴入於緩慢攪拌、稀釋的微溫(如130℉)明膠溶液而製備。此微溫的明膠溶液包在微滴的外圍,當明膠冷卻硬化後即形成一層明膠壁包裹著液體中心。
煙草粒自溶液中以標準化方法取出。
10g明膠和90g水混合並加熱至140℉以溶解明膠。加入20g煙草後倒入模具。強度可因以6g明膠和4g洋菜取代混合並加熱至190℉而增加。
表AS1列出製造可於口腔崩解的固化凝膠實施例的成分:
下表及說明顯示製造本發明不可溶凝膠(例如不於口中崩解的凝膠)之例示成分:
本組合物加入氯化鉀並完全混合後於180℉鑄型。
本組合物加入氯化鈣後於180℉鑄型。
本組合物加入硫酸鋁後於180℉鑄型。
416g之3.9%卡帕角叉菜膠溶液與51.0g煙草混合。攪拌加熱至180至190℉後倒入所需形狀之模具。冷卻後,由模具取出所得固形物並乾燥至所需的煙草濃度與膠體硬度。
於另一步驟中,於架設有攪拌機、攪拌棒、與加熱板之1000ml不鏽鋼容器中,加入200℉以上的400ml水。將水持續攪拌與加熱,於2分鐘內加入16.0g卡帕角叉菜膠(Gelcarin GP812,FMC Biopolymer)。繼續攪拌所得混合物20分鐘,或至卡帕角叉菜膠全部溶解後,將煙草加至均質溶液,且持續攪拌所得溶液2分鐘並維持180℉的最適溫度。劇烈攪拌下於溶液中加入0.8g蔗糖素粉末與7g肉桂油(Wixon Industries)。攪拌1分鐘後,快速以內徑0.5cm滴管轉置於Teflon覆蓋的金屬模具以獲得所需形狀。冷卻至室溫後,由模具移出所得凝膠並於室溫下風乾1小時至數日直到獲得所需凝膠硬度。
100g之20%明膠水溶液與33g煙草混合。攪拌加熱至140至150℉後倒入所需形狀之模具。在冰箱中視所需堅固程度冷卻數分鐘至數日後,由模具移出所得固體並乾燥至所需的煙草濃度與膠體硬度。
另一步驟中,於架設有攪拌機、攪拌棒。與加熱板之400ml不鏽鋼容器中,加入140℉的80ml水。將水持續攪拌與加熱,於2分鐘內加入20.0g明膠(Type A 250 Bloom 40網眼,Gum Technology),繼續攪拌5分鐘,或至明膠全部溶解後,於2分鐘內加入33g煙草。持續攪拌所得混合物1分鐘後,加入0.3g蔗糖素粉末與1g薄荷油(rectified,Blend SX0910001,Essex Labs),將混合物劇烈攪拌另外的1分鐘並維持於140℉的溫度。所得混合物以內徑0.5cm滴管轉置於Teflon覆蓋的金屬模具以獲得所需形狀。冷卻至室溫後,由模具移出所得膠體,將該凝膠置於40℉冷藏1小時至數日以獲得所需硬度。
4%海藻膠鈉(Keltone LV,International Specialty Products)溶液係將12g海藻膠鈉加至288g沸騰的水,持續攪拌且於熱板上使水加熱30分鐘或直到形成均質物(庫存溶液
A)。第二溶液之0.50M磷酸氫鈉溶液,係將33.5g磷酸氫鈉七水合物(disodium hydrogen phosphate heptahydrate)溶解在200ml溫水且攪拌所得混合物至鹽完全溶解,接著以水調整溶液至250ml。100g之0.50M磷酸氫鈉溶液中加入20g煙草並攪拌5分鐘(庫存溶液B)。50g之所得煙草漿狀物(庫存溶液B)中加上50ml5 4%海藻膠鈉(庫存溶液A),攪拌所得混合物5分鐘。為了調味,將0.2g蔗糖素粉末與0.80g薄荷油(rectified,Blend SX0910001,Essex Labs)加至所得之煙草/海藻膠鈉漿狀物(溶液C),且攪拌所得混合物2分鐘。
為了由溶液C製備凝膠粒,5%之氯化鈣水溶液係由將5g氯化鈣加入95g水攪拌至氯化鈣完全溶解而製備(溶液D)。溶液C經滴管於10英吋高度逐滴滴入溶液D。每一滴微滴的外塗覆在接觸溶液D時硬化,形成類似固態凝膠的外塗覆與液態中心而沉降於氯化鈣溶液。凝膠粒放置於氯化鈣中2至4分鐘,移出,且風乾數分鐘。
溶液D
本發明之組成物亦可製成消費單元。該單元可包裝為可食用或不可食用材料。在一具體例中,該消費單元包括煙草(例如無煙煙草)或煙草組成物,例如薄片、錠劑、粒狀物、粒狀物、或本文所述之其他煙草組合物;及包裝,例如袋狀物。在一具體例中,該包裝可作為黏著劑,與該組合物一起保持,例如保持各種錠劑、粒狀物、薄片等。或者,該包裝可封入(enclose)組合物,例如鬆的錠劑、粒狀物、薄片等。該組合物亦可包括液體,例如煙草漿狀物。該包裝可為或可不為口中可崩解者。口中可崩解包裝可用於封入水性或非水性液體。當水性液體與水溶性包裝一起使用時,該液體包括預防包裝溶解之試劑。例示試劑包括糖、鹽、及其他能充分結合水之親水性試劑,以降滴水活性至水不再可接觸及溶解水溶性包裝之程度。該包裝亦可封入可符合口或於口中維持其形狀之可鑄型煙草組合物。在一具體例中,口中可崩解包裝封入無煙煙草,例如乾燥煙或煙草,其為可溶性(例如小於80微米之粒徑)。口中可崩解無煙煙草組合物可導至消費部分包裝,該包裝係使用可食用膜(其可或可不含有煙草),根據目標技術製造,而於連續熱形成或平行形成/填充/密封設備或其他合適之包裝設備上形成。消費單元亦可含有兩種或兩種以上,個別包裝之煙草部分,例如所有皆含於較大包裝中,其中一個含有其他部分,或無任何部分含於另一個。當使用多個部分時,任兩者可具相同或相異之調味、著色、煙草型式、或崩解速率。
例示包裝材料包括基於配方之膜組合物所形成之膜,該配方例如HPMC、CMC、果膠、海藻膠、普路蘭、及其他市售之可
生存、可食用膜形成聚合物,例如本文所述者。其他包裝材料可包括由明膠、HPMC、澱粉/卡拉膠、或其他市售可得材料所製成之預成形膠囊。該等包裝材料可包括煙草成分。位為口中可崩解之包裝包括編織及不織布纖維;經塗覆或為塗覆紙材;或穿孔或多孔塑膠膜。包裝可為經著色者。例示消費單元包括藉使用於商用包裝之任何方法所形成者,例如發泡包裝或插槽包裝(例如在垂直型式/填充/封入包裝機器)。
以下說明提供用於製造本發明之消費單元之例示成分。
本發明之任何組合物皆可以膜或膠囊作成膠囊。該膠囊物可提供著色、安定性(例如儲存、持有或消費期間),或感官察覺特性(例如調味、甜味、嗅覺或口感)。該膠囊物亦可含有煙草。
構建真空形成工具,其具有一系列為直徑3/4th英吋及深3/8th英吋且成形為圓形之空孔。本文之薄膜可製備為含有及不含有煙草作為成分。以真空形成工具將該等薄膜導入真空形成機。該膜置於加熱單元且加熱至200℉的溫度。將該薄膜迅速至於真空形成工具,且以真空吸引使薄膜進入空孔。隨後冷卻薄膜設定成形。之後將煙草粉末置入各空孔。選擇製備為有或無煙草之第二層膜片(以潮濕感覺擦拭薄膜表面)且以水薄層塗覆以創造黏性的、黏著的表面。將該黏性表面至於其中各空孔以煙草產品填充之所形成薄片之上方。該薄片一起加壓以形成密合的消費單元。各空孔由真空所形成之薄片上切割而製造各單元。當單元至於口中,其中薄膜崩解且在口腔中釋出煙草。
無煙煙草顆粒或粉末,例如鼻煙,可置於水可崩解袋中。當置於口中在一特定期間後,袋會崩解。呆可含有單一用量之
煙草。亦可含有本文所述之其他添加物。一旦包裝崩解時,煙草亦可互相黏結為可鑄型之煙草塊。
可崩解袋可使用如本文所述之膜而形成。膜形成袋可使用市售包裝設備,例如垂直的成形/填充/密封機(例如插槽包裝機)、平行的成形/填充/密封機、流式包裝機、熱成形機(泡殼包裝機)、及習知其他設備。
無煙煙草顆粒或粉末可置於,由例如纖維、紙或塑膠薄膜之開放或高度多孔性包裝材料,而經積層為水溶性包裝薄膜所製成之袋中。該水溶性薄膜層對煙草內容物提供保護,且在儲存及持有期間預防煙草經由不溶性材料之開口篩出。一旦將袋置於口中,水溶性薄膜層惠溶解或崩解。
薄膜實施例N、O、P、及Q中之薄膜可用於製造含有煙草袋之煙草。約1英吋×1¼英吋之個別單元係由所製造薄膜片上切割。該單元以長側摺疊且使用脈衝封口機(Clamco Model 210-8E)加熱密封。所形成單元之一終端以相同方法密封。漿經調味之煙草顆粒位入所形成袋狀物之內部,最後密封再以相同方法將袋狀物密封。含煙草之袋狀物於口中界於20秒至1分鐘崩解,釋出袋狀物之內容物。
煙草可塗覆或包埋於不溶基質。於形成薄膜時煙草可經分散在配方之水溶液中形成漿狀物;該漿狀物可塗覆至不溶基質,或用以飽和多孔性不溶基質。該漿狀物可轉為可溶或不可溶凝膠,或其可簡便地經乾燥以形成塗覆。當此經塗覆/經飽和之不溶基質之部分置於口中時,經由溶解、咀嚼、或其他方法而釋出感官察覺成分。一具體例中,配方中之煙草係經導入
多孔性基質,例如具開口單元聚胺基甲酸酯發泡物或高蓬鬆(loft)不織布纖維。該不溶基質可完全置於口中,或可置於桿或其他把手上,而在消費期間保留部分於口外。另一具體例中,配方中之煙草與不相容液體混合(例如巴西棕櫚蠟(carnauba wax)於水中之分散液),置於模具,且快速冷卻以使相分離而使煙草漿狀物配置於蠟狀結構中。該等基質亦可為可咀嚼的。
用於保留煙草於不溶基質中之配方包括本文所述之任何形成聚合物之薄膜;本文所述之任何凝膠系統及本文所述之任何塗覆物質。
將形成如本文所述之含有精細研磨煙草之組合物之薄膜,使用以飽和聚開口單元聚胺基甲酸酯發泡物(Stephenson & Lawyer,Inc.Grand Rapids,MI)之小片(例如12英吋×12英吋×1英吋)。該經飽和發泡物置於金屬盤後移入175℉循環式實驗室哄箱1小時。當由烘箱移出發泡物時,含有煙草之組合物已經乾燥而形成均勻覆蓋聚胺基甲酸酯發泡物所有空隙之塗覆物。該經塗覆之發泡物切割為適於至入口中之尺寸(例如1英吋×1英吋×1英吋)。使用後,該聚胺基甲酸酯由口中移出、丟棄。
將形成如本文所述之含有精細研磨煙草之海藻膠鈉及蓋鹽凝膠之組合物,使用以飽和聚開口單元聚胺基甲酸酯發泡物(例如12英吋×12英吋×1英吋)。該海藻膠鈉係經維持於180℉以防止凝膠之預熟定型。將該熱海藻膠鹽凝膠倒至聚胺基甲酸酯發泡物後,置於金屬盤且快速於40℉冷藏庫中冷卻定型凝膠。隨後將該發泡物置入175℉實驗室烘箱10分鐘乾燥凝膠表
面及以凝膠乾種為準漿溼度含量減低至50%。部分乾燥凝膠填充聚胺基甲酸酯發泡物之空隙。該發泡物係經切割為小片及置於口中。不溶基質之凝膠之又一實施例係將該凝膠乾燥至低溼度含量(例如,以凝膠乾種為準為10%)而製得。含煙草凝膠於發泡基質中顯示堅固、橡皮狀質地而且置於口中咀嚼時復水(rehydrate)緩慢。使用後,該聚胺基甲酸酯發泡物由口中移出、丟棄。
如前所述,材料之薄膜或薄片可經包裝、擠出、吹模、或其他塑形而形成管狀物、吸管狀物、或其他中空狀物。例示之薄膜或薄片材料已於本文之薄膜段中說明。該中空狀物可為單一層或多層。當使用多層時,某些層含有煙草而其他層含有著色劑、調味劑、甜味劑或如本文所述之其他化合物。不同層可為持有期間之安定形而施用或於消費期間控制崩解。例如管狀物或吸管狀物之螺旋包裝中空狀物需要黏著劑(例如CMC或瓜爾膠(guar))以防止散開。多層裝空狀物知該等層可含有相同或相異之著色劑或調味劑,且該等層可以相同或相異之速率崩解。如同於薄膜中,煙草可配置於一層或多層或可配置於三明治排列之層間。該中空狀物亦可包括崩解劑或加速崩解劑。
上述之組合物可為中空或經填充。該填充物可包括煙草、調味劑、甜味劑、調味遮蔽劑、或著色劑。該填充物之調味劑或著色劑可與中空狀物者相同或相異。填充物典型為凝膠(固體或可流動者),旦亦可為機械性堅固的或可為粉末或其他產品型式所組成。例示填充材料包所述之凝膠。中空狀物亦可以組合物填充,該組合物崩解較該形狀快,基於崩解速率而於不同時間提供煙草。
一具體例中,煙草核心(例如經以煙草及配方所配方)可由單或雙輥擠出機擠出至共押出鑄模(coextrusion die)。分開
之單或雙輥擠出機中,水可溶,熱塑性外層(例如經以配方及調味劑配方)可導致共押出鑄模以製造經塗覆桿狀物。典型的熱塑性外層可基於以羥丙基纖維塑(HPC)配方而提供,其於界於220至370℉的溫度擠出。此外,堅固擠出煙草桿可成為核心而以包裝薄膜包圍。
在一實施例中,含有羥丙基纖維塑、煙草、調味劑及甜味劑之熱塑性配方可吹模以形成中空狀物。
在另一實施例中,本文所述之薄膜可額外使用於製造螺旋纏繞吸管狀物及/或桿狀物。由所製造之薄膜切割得約10英吋×¾英吋之薄膜條。切割相同尺寸之紙條且螺旋性地纏繞直徑3/16英吋之不鏽鋼軸。紙纏繞軸的末端以膠帶纏住。以相同方式將薄膜條螺旋性地纏繞,以1/16英吋重疊於每隔螺旋。薄膜條以30%阿拉伯膠溶液在各重疊處黏住其本身。此步驟以另外兩薄膜條重複。軸與新形成之螺旋纏繞薄膜吸管狀物/桿狀物,置於75℃送風定溫烘箱(VWR型號1330FM)中乾燥15分鐘。由烘箱移出後,螺旋纏繞之吸管物/桿狀物由軸移除,且紙”核心”由吸管物/桿狀物之內部移除。所得之吸管物/桿狀物切割為各種尺寸。
舉例而言,螺旋纏繞之吸管物/桿狀物產品使用含有煙草之實施例N.之棒狀/包紙狀/袋狀/真空成形經調味的薄膜製備。含有一層、兩層及三層之實施例N之薄膜之吸管狀物/桿狀物品由所述方法製備。當置於口中時,該吸管物/桿狀物於1至5分鐘期間逐漸崩解。
在另一實施例中,吸管物/桿狀物產品使用兩層實施例N之薄膜製備。第三層薄膜以實施例O之用於棒狀/包紙狀/袋狀之經調味/著色薄膜製備。實施例O之薄膜為紅色、經肉桂調味且不含煙草。當置於口中時,此吸管物/桿狀物於1至5分
鐘期間逐漸崩解。
在另一實施例中,吸管物/桿狀物產品使用三層實施例P之用於棒狀/包紙狀/袋狀之經蜜桃調味的薄膜製備。實施例P之薄膜含煙草粉末及蜜桃糊。該吸管狀物/桿狀物品由上述方法製備。當置於口中時,該吸管物/桿狀物於1至5分鐘期間逐漸崩解。
在又一實施例中,吸管物/桿狀物產品使用三層實施例N及實施例Q之薄膜製備。一層使用實施例N之含煙草薄膜製備。實施例Q製備之透明、白色薄膜之第二層以間距1/8th英吋纏繞於第一層薄膜。實施例N製備之含煙草薄膜之第三層再次以間距間距1/8th英吋纏繞於第二層。該吸管狀物/桿狀物品由上述方法製備。當置於口中時,該吸管物/桿狀物於1至5分鐘期間逐漸崩解。此影響係提供螺旋纏繞之吸管狀物/桿狀物具有條形外觀。當置於口中時,該吸管物/桿狀物於1至5分鐘期間逐漸崩解。
在另一實施例中,據友直靜範圍由1/8至1/4英吋之中空菸草吸管物,係以類似於實施例AQ之成形部件所使用之方法而製備;而製造吸管物係使用管型鑄模。該吸管物於口中崩解緩慢經約5至10分鐘期間。相似物件可以習知方法(例如共押出),以填充物製造。
本文所述之任何煙草組合物可以多種方式改質。舉例而言,組合物可經塗覆單層或多層。使用該塗覆之目的,例如為持有、崩解速率、口感及著色。例示塗覆包括HPMC。塗覆或裝飾圖案可使用習知方法而施用於薄膜表面,該等方法例如噴灑法(spraying)、刷布法(brushing)、翻滾塗覆法(roll coating)、刮柄澆鑄法(doctor bar casting)、狹槽塗覆法(slot coating)、突起塗覆法(extrusion coating)、熱溶析
出法(hot melt deposition)、存放顆粒(depositing particles)或薄片(flakes)及其他典型的方法。塗覆可為無光澤或有光澤。塗覆可含有如本文所述之著色、調味、甜味劑、或調味遮蔽劑。塗覆中之著色、調味、甜味劑、或調味遮蔽劑可與位於其下之之組合物相同或不同。此外,多層塗覆亦可含有相同或不同之著色、調味、甜味劑、或調味遮蔽劑。該塗覆亦可以與位於其下之組合物不同之速速率崩解。舉例而言,塗覆可較位於其下之組合物更快崩解,以提供調味或其他感官察覺成分之散開。口中崩解塗覆亦可置於口中不崩解之組合物上。口中不崩解之塗覆可置於口中崩解之組合物上,且該塗覆係經由如咀嚼而移除。塗覆亦可用於使用前預防組合物中揮發成分之蒸發以及預防組合物之機械性軟化。塗覆以可含有煙草。
圖案可印製於組合物表面。印製圖案亦包含輕灑或分散化合物於組合物表面。該圖案可為隨機或依設計,例如標誌圖案(logo)。所有習知印製方法皆可使用,例如膠印(offset)、彈性凸版印製油墨(flexographic)、凹版印製(gravure)、噴墨(ink jet)、雷射(laser)、掃描印製(screen printing)或其他典型的方法。該印製圖案可含有或不含有如本文所述之著色、調味、甜味劑、或調味遮蔽劑。該著色、調味、甜味劑、或調味遮蔽劑可與位於其下之組合物相同或不同。此外,多層圖案亦可含有相同或不同之著色、調味、甜味劑、或調味遮蔽劑。該印製圖案亦可含有煙草,例如1至99%,較佳為10至50%。以百分比或絕對值而言,該圖案可含有較位於其下之組合物多之煙草。
薄片亦可添加至如本文所述之組合物。薄片可混合至組合物、可位於組合物之空隙、或位於表面,例如以塗覆黏著。
薄片可含有或不含有如本文所述之著色、調味、甜味劑、或調味遮蔽劑。薄片中之著色、調味、甜味劑、或調味遮蔽劑
可與位於其下之組合物相同或不同。此外,多種薄片亦可含有相同或不同之著色、調味、甜味劑、或調味遮蔽劑。薄片亦可含有煙草,例如多至99%,較佳為多至50%。薄片可由如本文所述之標準薄膜形成技術製得。以百分比或絕對值而言,該薄片可含有較位於其下之組合物多之煙草。
一旦該經印製、經塗覆、或經裝飾之薄膜製得時,可施用另外一層薄膜以塗覆、保護及密封該經印製、經涂婦或裝飾之表面。
本發明之組合物可成形為多種形式,例如植物及幾何形式(例如圓形、正方形、長方形、三角形、卵形、橢圓形等)。此外,組合物於表面可含有立體圖案(正向或負向)。該圖案可經設計,例如標誌圖案。
複合組合物(composite composition),亦即包括兩種或兩種以上之如本文所述之不同型產品,亦為本發明之目的。舉例而言,成形部件可含有凝膠組合物區域,例如具有多種調味。另一實施例中,錠劑可經凝膠圍繞。複合組合物亦可有不同崩解速率。
個別組合物會依該組合物之內容物而合宜的包裝。較佳地,該組合物係儲存於防水容器且於40及120℉間安定。儲存時,組合物典型地為乾的、可撓的、且無黏著性的。或者,組合物可於每份量間使用例如塑膠膜或紙無黏性柵欄物加以包裝。組合物以可以大量型式提供,而其中之每份量係經隔開的。
另一具體例中,該包裝為水不滲透性且水不溶性,及煙草(例如為液體、漿狀物、或可流動凝膠形式)係分散於包裝(例如可擠壓之塑膠包裝、風箱、或噴霧瓶),且能由包裝分散至口中。該風箱可壓縮用於口服使用。溶液或漿狀物製備用於塑膠風箱容器或其他類似消耗包裝容器,其中該液體藉擠壓射至
口中。觸變性(thixotropic)聚合物結合煙草及其他成分而製備合適用於其他容器之高黏度溶液。煙草顆粒可為較大尺寸,但仍需夠小已能通過該容器開口。噴霧瓶中含有安定煙草漿狀物;煙草顆粒係尺寸化為能安定的通過噴嘴而不組閣其開口者;及該煙草漿狀物係直接噴霧至口腔。液體噴霧係經由於水中溶解例如黃原膠、結冷膠或右懸膠,且將煙草顆粒懸浮於低黏度(例如小於50厘泊)溶液。其他化合物,例如調味劑、甜味劑及分散劑可加至該溶液。該煙草顆粒研磨至顆粒尺寸而使均質溶液通過噴霧容器之開口。其它包裝可使用其他擠壓方法將菸草逐出至口中。
下列煙草溶液可包括於本文所述之任何組合物。
混合0.2克黃原膠(Kelzan來自C.P.Kelco)於78.6克冷水,劇烈攪拌30分鐘製備溶液。於持續劇烈攪拌下,添加20克精細研磨煙草、0.2克蔗糖素、及2克肉桂調味劑至此溶液。此溶液黏度以水調整至50厘泊之黏度。
混合1克黃原膠(Kelzan來自C.P.Kelco)於78.6克冷水,劇烈攪拌30分鐘製備溶液。於持續劇烈攪拌下,添加20克精細研磨煙草、0.2克蔗糖素、及2克肉桂調味劑至此溶液。溶液黏度為1,500厘泊。
添加2克中等黏度之羧甲基纖維素(CMC 7MF來自Hercules,Inc.)至35.8克冷水及40克甘油之混合物,劇烈攪拌30分鐘製備糊狀物。添加20克精細煙草、0.2克蔗糖素、及2克肉桂調味劑至此混合物。製備為高剪力敏感之濃糊狀物。此糊狀物可導入管或其他可擠壓包裝,此處由擠壓之剪力會減低黏度而
使糊狀物流出。
本發明中特定具體例之揭示係用於說明目的。而不意味徹底地或限制本發明之範圍於本文所述之特定形式。雖然本發明參考數個具體例而加以說明,但此項技術領域中具有通常知識者當知,如申請專利範圍所述,可加以進行各種變化而不悖離本發明之精神及範疇。所有出現於本文之專利、專利公開及公告皆合併於此作為參考文獻。
其他具體例於申請專利範圍中。
Claims (25)
- 一種可在口中崩解的無煙煙草產品,包括一薄膜,該薄膜包括煙草及一水溶性高分子,其中該煙草的平均粒徑為250μm或更小。
- 如申請專利範圍第1項所述之無煙煙草產品,包括一單層。
- 如申請專利範圍第1項所述之無煙煙草產品,其中該薄膜於2分鐘內崩解。
- 如申請專利範圍第1項所述之無煙煙草產品,其中該薄膜的厚度小於500μm。
- 如申請專利範圍第1項所述之無煙煙草產品,其中該薄膜的厚度介於5至250μm。
- 如申請專利範圍第1項所述之無煙煙草產品,其中更包括一甜味劑。
- 如申請專利範圍第6項所述之無煙煙草產品,其中該甜味劑係包括蔗糖、蔗糖素、乙醯磺胺酸鉀(acesulfame potassium)、阿斯巴甜、甜精、糖精、乳糖、葡萄糖、果糖、山梨醇、或甘露醇。
- 如申請專利範圍第1項所述之無煙煙草產品,其中更包括一界面活性劑。
- 如申請專利範圍第1項所述之無煙煙草產品,其中更包括一增塑劑。
- 如申請專利範圍第9項所述之無煙煙草產品,其中該增 塑劑係包括甘油、丙二醇、聚乙二醇、山梨醇/甘露醇、乙醯化甘油酯、三乙酸酯、或1,3-丁二醇。
- 如申請專利範圍第1項所述之無煙煙草產品,其中更包括一微結晶纖維素。
- 如申請專利範圍第1項所述之無煙煙草產品,其中更包括卵磷脂、硬脂酸甘油、或硬脂酸聚乙二醇。
- 如申請專利範圍第1項所述之無煙煙草產品,其中更包括包括羥丙基纖維素(HPC)、羥丙基甲基纖維素(HPMC)、果膠、瓜爾豆膠、黃原膠、刺槐豆膠、阿拉伯樹膠、海藻膠鹽、依而他角叉菜膠、或羅望子膠。
- 如申請專利範圍第13項所述之無煙煙草產品,其中更包括20%至45%的羥丙基纖維素(HPC)及羥丙基甲基纖維素(HPMC)。
- 如申請專利範圍第1項所述之無煙煙草產品,其中更包括一調味劑,擇自下列所組成之群組:薄荷腦、肉桂、冬青、蜜桃、綠薄荷、薄荷、或薄荷油。
- 如申請專利範圍第1項所述之無煙煙草產品,其中該煙草的平均粒徑為100μm或更小。
- 如申請專利範圍第1項所述之無煙煙草產品,其中該煙草的平均粒徑為80μm或更小。
- 如申請專利範圍第1項所述之無煙煙草產品,其中該煙草的平均粒徑為75μm或更小。
- 如申請專利範圍第1項所述之無煙煙草產品,其中該煙 草的平均粒徑為50μm或更小。
- 如申請專利範圍第1項所述之無煙煙草產品,其中該煙草的平均粒徑為25μm或更小。
- 如申請專利範圍第1項所述之無煙煙草產品,其中該煙草的平均粒徑為20μm或更小。
- 如申請專利範圍第1項所述之無煙煙草產品,包括1%至80%的煙草。
- 如申請專利範圍第1項所述之無煙煙草產品,包括1%至50%的煙草。
- 如申請專利範圍第1項所述之無煙煙草產品,包括1%至40%的煙草。
- 如申請專利範圍第1項所述之無煙煙草產品,包括20%至40%的煙草。
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- 2004-11-05 WO PCT/US2004/036793 patent/WO2005046363A2/en active Application Filing
- 2004-11-05 CN CN201210162595.1A patent/CN102669810B/zh not_active Expired - Fee Related
- 2004-11-05 JP JP2006539648A patent/JP4931596B2/ja not_active Expired - Fee Related
- 2004-11-05 AU AU2004289248A patent/AU2004289248B2/en not_active Ceased
- 2004-11-05 US US10/982,248 patent/US8469036B2/en active Active
- 2004-11-05 BR BRPI0415741-9B1A patent/BRPI0415741B1/pt not_active IP Right Cessation
- 2004-11-05 EP EP04800749A patent/EP1691631A4/en not_active Withdrawn
- 2004-11-05 CN CN201410462828.9A patent/CN104397869B/zh not_active Expired - Lifetime
- 2004-11-08 TW TW093133982A patent/TWI428093B/zh not_active IP Right Cessation
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2007
- 2007-11-08 HK HK13103320.0A patent/HK1175963A1/zh unknown
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- 2008-12-29 US US12/345,012 patent/US8636011B2/en active Active
- 2008-12-29 US US12/345,063 patent/US10765140B2/en not_active Expired - Lifetime
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- 2012-02-10 US US13/370,586 patent/US10098376B2/en active Active
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Also Published As
Publication number | Publication date |
---|---|
JP2007515950A (ja) | 2007-06-21 |
US8469036B2 (en) | 2013-06-25 |
US10098376B2 (en) | 2018-10-16 |
CN102669810A (zh) | 2012-09-19 |
US10765140B2 (en) | 2020-09-08 |
JP5455131B2 (ja) | 2014-03-26 |
EP1691631A4 (en) | 2012-09-05 |
JP4931596B2 (ja) | 2012-05-16 |
WO2005046363A2 (en) | 2005-05-26 |
BRPI0415741B1 (pt) | 2013-07-23 |
US8636011B2 (en) | 2014-01-28 |
JP2012085643A (ja) | 2012-05-10 |
US20090133704A1 (en) | 2009-05-28 |
TW200529772A (en) | 2005-09-16 |
BRPI0415741A (pt) | 2006-12-19 |
CN102669810B (zh) | 2014-11-05 |
WO2005046363A3 (en) | 2006-11-16 |
CN104397869B (zh) | 2016-06-08 |
CN104397869A (zh) | 2015-03-11 |
US20120199149A1 (en) | 2012-08-09 |
HK1175963A1 (zh) | 2013-07-19 |
AU2004289248B2 (en) | 2012-05-03 |
US20050244521A1 (en) | 2005-11-03 |
EP1691631A2 (en) | 2006-08-23 |
AU2004289248A1 (en) | 2005-05-26 |
US20190029313A1 (en) | 2019-01-31 |
US20090133703A1 (en) | 2009-05-28 |
US20200329755A1 (en) | 2020-10-22 |
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