EP0235539A2 - Process for flavouring tabacco - Google Patents
Process for flavouring tabacco Download PDFInfo
- Publication number
- EP0235539A2 EP0235539A2 EP87100873A EP87100873A EP0235539A2 EP 0235539 A2 EP0235539 A2 EP 0235539A2 EP 87100873 A EP87100873 A EP 87100873A EP 87100873 A EP87100873 A EP 87100873A EP 0235539 A2 EP0235539 A2 EP 0235539A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- tobacco
- water
- emulsion
- flavoring
- flavoring substance
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
Definitions
- the tobacco industry uses the use of different flavoring substances in order to improve the organoleptic qualities of the different kinds of products of varied plant origin that it has to process.
- US Pat. No. 3,550,598 describes a process which consists in spraying a suspension of water-soluble capsules containing the flavoring substance on the tobacco product to be flavored. Such a process has been applied in particular to the manufacture of reconstituted tobacco leaves using less noble cuts, powders or ribs, originating from the treatment of the leaves.
- US Pat. No. 3,623,489 describes a process for the flavoring of tobacco which consists in adhering to tobacco cups or reconstituted leaves of microcapsules containing a volatile flavoring substance.
- Microcapsules have the property of bursting under the effect of heat, as it is released, for example when lighting or smoking a cigarette, to release the active volatile components of the aroma, generally of eugenol.
- the aforementioned US patent suggests that microcapsules can be obtained by any ordinary encapsulation method.
- the volatile flavoring substance is first retained on the surface of the tobacco leaves or particles by adhesion of the emulsion due to the binding effect exerted by the support substance. Under the effect of the ensuing drying, which is carried out by simple gradual exposure of the tobacco thus treated to the air or by the use of a heat source, if necessary by applying a slight suction or ventilation , the flavoring substance is retained in the form of small droplets coated with a water-soluble protective layer constituted by the support which is now dry.
- polyvinyl acetate PVA
- polyvinyl alcohol dextrins (natural or modified), starch (natural or modified), vegetable gums, proteins (natural or alginates, carrageenans, pectins, xanthans or cellulose derivatives such as, for example, carboxymethylcellulose, methylcellulose, hydroxymethylcellulose.
- proteins naturally or alginates, carrageenans, pectins, xanthans or cellulose derivatives such as, for example, carboxymethylcellulose, methylcellulose, hydroxymethylcellulose.
- gum arabic, shellac, maltodextrins, starch or partially hydrolysed proteins are used.
- emulsifying agent mono- or diglycerides of fatty acids, esters of fatty acids with sorbitol or saccharides or esters of tartaric, citric, ascorbic or lactic acid can be used.
- the process of the invention is carried out by spraying an emulsion and for this purpose a spray nozzle is used, for example with compressed air. It is of course possible to vary the pressure as a function of the viscosity of the emulsion, of the desired flow rate and of the product which it is desired to flavor. A pressure between 2 and 10 bar, preferably 3 to 5 bar, seems to be perfectly suited to the different cases examined.
- a nozzle of the Venturi type with compressed air at 4 bar is used, with an air nozzle with a diameter of 4 to 8 mm, a liquid suction nozzle of 0.6- 0.9 mm and an emulsion flow rate of 10 to 40 g / minute.
- the application of the emulsion to the product to be treated can be done by placing the product on a flat surface, for example, by spreading it on a rolling belt or in a rotary drum, which makes it possible to obtain a very coating. homogeneous tobacco.
- the water brought by the spray of the emulsion on the tobacco is absorbed or evaporates quickly at room temperature, which makes drying unnecessary. If the emulsion however were to add to tobacco quantities of water greater than 10-15%, drying in an oven of treated tobacco at around 40 ° C for 10 to 20 minutes may be necessary.
- the process of the invention has certain advantages over known methods of flavoring tobacco.
- the process of the invention can be applied just as well to the flavoring of tobacco of natural origin as to that of artificial tobacco.
- the spraying of the emulsion can take place during any phase of the tobacco treatment, either on the leaves or on sections.
- the flavoring compositions generally used can be used to impart, improve or modify the taste and aroma of tobacco. If necessary, it is of course possible to use specific aromatic substances isolated, such as menthol or eugenol. Among the useful volatile substances which can be used for this purpose, mention should be made of those described in patent FR 2,175,236. Their concentrations in the emulsion depend on the nature of the product to be treated, as well as on the particular aromatic effect that is sought. Concentrations of the order of 10 to 100-200 ppm (parts per million) by weight, based on the weight of flavored tobacco, can generally be used in most practical cases.
- the viscosity of this mixture is 72 cps.
- a flavoring composition of Virginia tabac type (origin: Firmenich SA, Geneva: Tabac 53.476) was incorporated at a rate of 0.5% by weight into the emulsion described in Example 1.
- the panel of experts was able to determine that the aroma developed by the "test" cigarettes had a richer note, while the acrid and irritant character specific to tobacco was lessened.
- a flavoring composition of the fruity type for tobacco (origin: Firmenich SA, Geneva: Tobacco 53.911) particularly suitable for flavoring tobacco (mixture of "flue-” and “air-cured” type tobacco with oriental tobacco) manufacture of kreteks (Indonesian type cigarettes) was incorporated at a rate of 1% by weight in the emulsion described in Example 1. The manufacture of “test” and “control” cigarettes as well as the evaluation of their smoke been performed as described above.
- test cigarettes developed a marked fruity character of ripe banana, with a light hint of dry fruit.
- Example 1 “Test” and "control” cigarettes were then prepared as shown in Example 1. The evaluation by an expert group indicated that the smoke from the "test” cigarettes had a dry fruit character. and a slightly caramel note.
- test and control cigarettes were prepared which were then subjected to evaluation (see previous examples).
- the expert group reported that smoke from "test” cigarettes had a dry fruit character and a typical aroma of ripe banana.
- the smoke developed by the "test” cigarettes was also less irritating thanks to its more fruity base note.
- a flavoring composition for “kretek” type cigarettes consisting essentially of eugenol, was added, at a rate of 8% by weight, to an emulsion prepared according to the method indicated in Example 5. the flavoring of a tobacco mixture, as indicated in Example 1, and then conducts the organoleptic evaluation on the cigarettes obtained by comparison with “control” cigarettes flavored by spraying on the same type of tobacco of a alcoholic solution (95% ethyl alcohol) with the same aroma.
- test cigarettes developed a smoke whose aroma was more complete while having a better power of diffusion.
- Example 5 A 20% by weight solution of menthol in a 1: 1 mixture of ethanol / propylene glycol was incorporated into the emulsion described in Example 5 in an amount of 25 parts of menthol solution per 100 parts of emulsion. Following the method described in Example 1, an American blend of tobacco was then flavored, using 100 g of flavoring emulsion per 1 kg of tobacco.
- the flavored tobacco was then left to stand for 8 weeks, then it was used to manufacture "test” cigarettes, the smoke of which was subjected to organoleptic evaluation by comparison with that developed by "control” cigarettes obtained by flavoring. using an alcoholic solution of the same aroma in 95% alcohol.
- the flavor of the “test” cigarettes is entirely comparable to that obtained by the use of the emulsion according to Example 5.
- the emulsion was prepared as follows: In a suitable container, the water was stirred slowly using a magnetic stirrer or a propeller stirrer. The solid components formed by the water-soluble support (such as starch, dextrins or alginate) were added slowly in small portions. The medium is then left to swell and dissolve at room temperature, after which the emulsifier first and the aroma then have been added to the aqueous solution kept stirring until a homogeneous and fine emulsion is obtained.
- a suitable container the water was stirred slowly using a magnetic stirrer or a propeller stirrer.
- the solid components formed by the water-soluble support such as starch, dextrins or alginate
- the medium is then left to swell and dissolve at room temperature, after which the emulsifier first and the aroma then have been added to the aqueous solution kept stirring until a homogeneous and fine emulsion is obtained.
Landscapes
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Tobacco Products (AREA)
Abstract
On décrit un procédé d'aromatisation du tabac consistant en le giclement d'une émulsion constituée par une substance aromatisante active non-miscible à l'eau, une solution aqueuse d'un support hydrosoluble et un agent émulsifiant sur des feuilles ou particules de tabac.A method of flavoring tobacco is described, consisting of the spraying of an emulsion consisting of an active flavoring substance immiscible with water, an aqueous solution of a water-soluble support and an emulsifying agent on tobacco leaves or particles. .
Ce procédé est plus avantageux que celui, traditionnel, qui consiste en le giclement d'une solution alcoolique de la substance aromatisante même. This process is more advantageous than the traditional one, which consists of spurting an alcoholic solution of the flavoring substance itself.
Description
Selon une pratique courante, l'industrie du tabac a recours à l'utilisation de différentes substances aromatisantes afin d'améliorer les qualités organoleptiques des différentes sortes de produits d'origine végétale variée qu'elle a à traiter.According to current practice, the tobacco industry uses the use of different flavoring substances in order to improve the organoleptic qualities of the different kinds of products of varied plant origin that it has to process.
Diverses techniques d'aromatisation ont été proposées par le passé. Toutefois, l'industrie a recours presque exclusivement à deux techniques traditionnelles: le trempage du tabac dans une solution appropriée, généralement aqueuse, de la substance aromatisante ou le giclement de cette solution sur le tabac même.Various flavoring techniques have been proposed in the past. However, the industry almost exclusively uses two traditional techniques: soaking the tobacco in a suitable solution, usually an aqueous solution, of the flavoring substance or spraying this solution on the tobacco itself.
Le désavantage principal de ces techniques est que les composants aromatiques actifs possèdent pour la plupart une tension de vapeur appréciable déjà à température ambiante et, de ce fait, ils s'évaporent et s'échappent plus ou moins rapidement de la surface du produit traité.The main disadvantage of these techniques is that the active aromatic components for the most part have an appreciable vapor pressure already at room temperature and, therefore, they evaporate and escape more or less quickly from the surface of the treated product.
Pour pallier ce désavantage, diverses techniques d'encapsulation ont été proposées. Le brevet US 3,550,598 décrit un procédé qui consiste à gicler une suspension de capsules hydrosolubles renfermant la substance aromatisante sur le produit de tabac à aromatiser. Un tel procédé a été appliqué en particulier à la manufacture de feuilles de tabac reconstituées utilisant des coupes moins nobles, poudres ou nervures, provenant du traitement des feuilles.To overcome this disadvantage, various encapsulation techniques have been proposed. US Pat. No. 3,550,598 describes a process which consists in spraying a suspension of water-soluble capsules containing the flavoring substance on the tobacco product to be flavored. Such a process has been applied in particular to the manufacture of reconstituted tobacco leaves using less noble cuts, powders or ribs, originating from the treatment of the leaves.
Le brevet US 3,623,489 décrit un procédé pour l'aromatisation du tabac qui consiste à faire adhérer à des coupes de tabac ou des feuilles reconstituées des microcapsules renfermant une substance aromatisante volatile. Les microcapsules ont la propriété d'éclater sous l'effet de la chaleur, telle qu'elle se dégage par exemple lorsqu'on allume ou que l'on fume une cigarette, pour libérer les composants volatils actifs de l'arôme, généralement de l'eugénol. Le brevet US susmentionné suggère que les microcapsules peuvent être obtenues par n'importe quelle méthode d'encapsulation ordinaire.US Pat. No. 3,623,489 describes a process for the flavoring of tobacco which consists in adhering to tobacco cups or reconstituted leaves of microcapsules containing a volatile flavoring substance. Microcapsules have the property of bursting under the effect of heat, as it is released, for example when lighting or smoking a cigarette, to release the active volatile components of the aroma, generally of eugenol. The aforementioned US patent suggests that microcapsules can be obtained by any ordinary encapsulation method.
D'autres techniques d'aromatisation du tabac ont été suggérées mais n'ont guère rencontré jusqu'ici un intérêt majeur. Parmi celles-ci, on peut mentionner l'adjonction d'arôme à un élément polymérique destiné à être incorporé dans un filtre à cigarette (brevet US 3,603,319) ou l'utilisation d'une résine échangeuse cationique ou anionique pouvant se combiner avec certaines molécules d'agent aromatisant basique ou acide (brevet US 3,280,823).Other tobacco flavoring techniques have been suggested but have so far met with no major interest. Among these, mention may be made of the addition of flavor to a polymeric element intended to be incorporated into a cigarette filter (US patent 3,603,319) or the use of a cationic or anionic exchange resin which can be combined with certain molecules. basic or acidic flavoring agent (US Patent 3,280,823).
L'art antérieur est riche en exemples spécifiques concernant l'aromatisation d'aliments par microencapsulation. Parmi les procédés récemment rendus publics, il convient de citer ceux décrits dans la demande de brevet européen 11324, le brevet US 4,339,422 et le brevet européen 70719. Ces documents décrivent des procédés pour la préparation de microcapsules par des méthodes ayant recours à la technique dite du lit fluidisé. Plus particulièrement, le brevet européen 70719 décrit un procédé d'encapsulation de liquides volatils, lequel procédé consiste à gicler une suspension contenant le liquide volatil et une solution d'un support approprié sur des particules solides, poudres ou écailles, mises en agitation dans un mélangeur à lit fluidisé. Il se forme ainsi des capsules renfermant le liquide volatil actif, lesquelles capsules peuvent être ensuite utilisées pour l'aromatisation de produits de consommation selon l'une des méthodes connues.The prior art is rich in specific examples concerning the flavoring of food by microencapsulation. Among the processes recently made public, mention should be made of those described in European patent application 11324, US patent 4,339,422 and European patent 70719. These documents describe processes for the preparation of microcapsules by methods using the technique known as of the fluidized bed. More particularly, European patent 70719 describes a process for encapsulating volatile liquids, which process consists in spraying a suspension containing the volatile liquid and a solution of an appropriate support on solid particles, powders or scales, stirred in a fluidized bed mixer. Capsules containing the active volatile liquid are thus formed, which capsules can then be used for flavoring consumer products according to one of the known methods.
Nous avons maintenant découvert qu'il était possible de procéder à l'aromatisation directe de tabac, sous forme de feuilles, poudres, particules ou film, par un procédé simple qui consiste à mettre en contact une substance aromatisante volatile active non-miscible à l'eau avec les feuilles ou particules de tabac, le contact étant obtenu par giclement direct sur leur surface exposée d'une émulsion obtenue par mélange de la substance aromatisante avec une solution aqueuse d'un support hydrosoluble en présence d'un agent émulsifiant.We have now discovered that it is possible to carry out the direct flavoring of tobacco, in the form of leaves, powders, particles or film, by a simple process which consists in bringing into contact an active volatile flavoring substance immiscible with l water with tobacco leaves or particles, contact being obtained by direct spraying on their exposed surface with an emulsion obtained by mixing the flavoring substance with an aqueous solution of a water-soluble support in the presence of an emulsifying agent.
La substance aromatisante volatile est d'abord retenue à la surface des feuilles ou particules de tabac par adhésion de l'émulsion grâce à l'effet de liaison exercée par la substance de support. Sous l'effet du séchage qui s'ensuit, et qui s'effectue par simple exposition graduelle du tabac ainsi traité à l'air ou par l'emploi d'une source de chaleur, le cas échéant en appliquant une légère aspiration ou ventilation, la substance aromatisante est retenue sous forme de petites gouttelettes enrobées d'une couche protectrice hydrosoluble constituée par le support désormais sec.The volatile flavoring substance is first retained on the surface of the tobacco leaves or particles by adhesion of the emulsion due to the binding effect exerted by the support substance. Under the effect of the ensuing drying, which is carried out by simple gradual exposure of the tobacco thus treated to the air or by the use of a heat source, if necessary by applying a slight suction or ventilation , the flavoring substance is retained in the form of small droplets coated with a water-soluble protective layer constituted by the support which is now dry.
Il s'agit en l'occurrence d'un procédé simple qui ne nécessite pas l'emploi d'un appareillage particulier, tel que pourrait l'être un atomiseur ou un mélangeur à lit fluidisé. L'opération a d'ailleurs lieu à température ambiante, ce qui se traduit par une économie d'énergie par rapport aux méthodes mentionnées. Dans la plupart des cas, il n'est même pas nécessaire de procéder au séchage du tabac, la quantité d'eau utilisée pour la préparation de l'émulsion étant absorbée entièrement par le tabac afin de le maintenir au taux d'humidité requis.This is a simple process which does not require the use of any particular apparatus, such as an atomizer or a fluidized bed mixer. The operation also takes place at room temperature, which results in energy savings compared to the methods mentioned. In most cases, it is not even necessary to dry the tobacco, the amount of water used for the preparation of the emulsion being absorbed entirely by the tobacco in order to maintain it at the required humidity level.
A titre de support hydrosoluble, on peut utiliser l'acétate de polyvinyle (PVA), l'alcool polyvinylique, des dextrines (naturelles ou modifiées), de l'amidon (naturel ou modifié), des gommes végétales, des protéines (naturelles ou modifiées), des alginates, des carragénanes, des pectines, des xanthanes ou des dérivés de la cellulose telles par exemple la carboxyméthylcellulose, la méthylcellulose, l'hydroxyméthylcellulose. Ces supports hydrosolubles peuvent être employés séparément ou en mélange. A titre préférentiel, on utilise la gomme arabique, la gomme laque, les maltodextrines, l'amidon ou des protéines partiellement hydrolysées.As water-soluble support, polyvinyl acetate (PVA), polyvinyl alcohol, dextrins (natural or modified), starch (natural or modified), vegetable gums, proteins (natural or alginates, carrageenans, pectins, xanthans or cellulose derivatives such as, for example, carboxymethylcellulose, methylcellulose, hydroxymethylcellulose. These water-soluble supports can be used separately or as a mixture. Preferably, gum arabic, shellac, maltodextrins, starch or partially hydrolysed proteins are used.
A titre d'agent émulsifiant, on peut utiliser des mono- ou diglycérides d'acides gras, des esters d'acides gras avec le sorbitol ou les saccharides ou des esters d'acide tartrique, citrique, ascorbique ou lactique.As emulsifying agent, mono- or diglycerides of fatty acids, esters of fatty acids with sorbitol or saccharides or esters of tartaric, citric, ascorbic or lactic acid can be used.
Le procédé de l'invention s'effectue par giclement d'une émulsion et à cet effet on a recours à un gicleur, par exemple à air comprimé. On peut bien entendu varier la pression en fonction de la viscosité de l'émulsion, du débit désiré et du produit que l'on désire aromatiser. Une pression comprise entre 2 et 10 bar, de préférence de 3 à 5 bar, semble être parfaitement adaptée aux différents cas examinés.The process of the invention is carried out by spraying an emulsion and for this purpose a spray nozzle is used, for example with compressed air. It is of course possible to vary the pressure as a function of the viscosity of the emulsion, of the desired flow rate and of the product which it is desired to flavor. A pressure between 2 and 10 bar, preferably 3 to 5 bar, seems to be perfectly suited to the different cases examined.
Selon un mode préférentiel d'exécution, on utilise un gicleur du type Venturi à air comprimé à 4 bar, avec une buse d'air d'un diamètre de 4 à 8 mm, une buse d'aspiration du liquide de 0,6-0,9 mm et un débit d'émulsion de 10 à 40 g/minute.According to a preferred embodiment, a nozzle of the Venturi type with compressed air at 4 bar is used, with an air nozzle with a diameter of 4 to 8 mm, a liquid suction nozzle of 0.6- 0.9 mm and an emulsion flow rate of 10 to 40 g / minute.
L'application de l'émulsion sur le produit à traiter peut se faire en disposant le produit sur une surface plane, par exemple, en l'étalant sur une bande roulante ou dans un tambour rotatif, ce qui permet d'obtenir un enrobage très homogène du tabac.The application of the emulsion to the product to be treated can be done by placing the product on a flat surface, for example, by spreading it on a rolling belt or in a rotary drum, which makes it possible to obtain a very coating. homogeneous tobacco.
Comme indiqué plus haut, l'eau apportée par le giclement de l'émulsion sur le tabac est absorbée ou s'évapore rapidement à température ambiante, ce qui rend un séchage superflu. Si l'émulsion toutefois devait ajouter au tabac des quantités d'eau supérieures à 10-15%, un séchage à l'étuve du tabac traité à environ 40°C pendant 10 à 20 minutes pourrait s'avérer nécessaire.As indicated above, the water brought by the spray of the emulsion on the tobacco is absorbed or evaporates quickly at room temperature, which makes drying unnecessary. If the emulsion however were to add to tobacco quantities of water greater than 10-15%, drying in an oven of treated tobacco at around 40 ° C for 10 to 20 minutes may be necessary.
Les proportions pondérales respectives des différents ingrédients de l'émulsion peuvent varier dans une gamme de valeurs assez étendue. De préférence, elles sont
- a. de 0,5% à 20% pour la substance aromatisante volatile active,
- b. de 5% à 30% pour le support hydrosoluble,
- c. de 0,1% à 10% pour l'agent émulsifiant, et
- d. pour le restant d'eau.
- at. from 0.5% to 20% for the active volatile flavoring substance,
- b. from 5% to 30% for the water-soluble support,
- vs. from 0.1% to 10% for the emulsifying agent, and
- d. for the rest of the water.
Le procédé de l'invention présente des avantages certains par rapport aux méthodes connues d'aromatisation du tabac.The process of the invention has certain advantages over known methods of flavoring tobacco.
Il s'agit en effet d'une méthode "directe" qui ne fait pas appel aux techniques d'encapsulation indirecte d'arôme connues dans l'art. Le procédé est donc plus économique. Comparé aux méthodes traditionnelles pratiquées dans l'industrie du tabac, telle l'aspersion de l'arôme sous forme de solution alcoolique, le procédé de l'invention se révèle être plus efficace et plus fiable. La dispersion des constituants volatiles de l'arôme dans l'atmosphère environnante pendant l'opération de giclement est moindre, ce qui entraîne d'une part une moindre perte de l'arôme et d'autre part, une aromatisation plus équilibrée, le rapport respectif des différents constituants de l'arôme restant pratiquement constant pendant toute l'opération. Enfin, le tabac ainsi aromatisé conserve pendant longtemps les propriétés organoleptiques acquises sans se dénaturer, l'arôme étant à l'abri des influences et agents extérieurs (telle l'évaporation ou l'oxydation) qui pourraient en modifier le caractère propre.It is indeed a "direct" method which does not call upon the techniques of indirect aroma encapsulation known in the art. The process is therefore more economical. Compared to the traditional methods practiced in the tobacco industry, such as the spraying of the aroma in the form of an alcoholic solution, the process of the invention proves to be more effective and more reliable. The dispersion of the volatile constituents of the aroma in the surrounding atmosphere during the spraying operation is less, which results on the one hand in a less loss of the aroma and on the other hand, a more balanced aromatization, the ratio respective of the different constituents of the aroma remaining practically constant throughout the operation. Finally, the tobacco thus flavored retains the organoleptic properties acquired for a long time without denaturing, the aroma being protected from external influences and agents (such as evaporation or oxidation) which could modify its own character.
Le procédé de l'invention peut s'appliquer tout aussi bien à l'aromatisation de tabac d'origine naturelle qu'à celle de tabac artificiel. Le giclement de l'émulsion peut s'effectuer pendant n'importe quelle phase du traitement de tabac, soit sur les feuilles, soit sur des coupes.The process of the invention can be applied just as well to the flavoring of tobacco of natural origin as to that of artificial tobacco. The spraying of the emulsion can take place during any phase of the tobacco treatment, either on the leaves or on sections.
A titre de substance aromatisante active, on peut employer les compositions aromatisantes généralement utilisées pour conférer, améliorer ou modifier le goût et l'arôme de tabac. Le cas échéant, on peut bien entendu utiliser des substances aromatiques spécifiques isolées, tel le menthol ou l'eugénol. Parmi les substances volatiles utiles qui peuvent être employées à cet effet, il convient de mentionner celles décrites dans le brevet FR 2.175.236. Leurs concentrations dans l'émulsion dépendent de la nature du produit à traiter, ainsi que de l'effet aromatique particulier que l'on recherche. Des concentrations de l'ordre de 10 à 100-200 ppm (parties par million) en poids, par rapport au poids du tabac aromatisé peuvent généralement être employées dans la plupart des cas pratiques.As active flavoring substance, the flavoring compositions generally used can be used to impart, improve or modify the taste and aroma of tobacco. If necessary, it is of course possible to use specific aromatic substances isolated, such as menthol or eugenol. Among the useful volatile substances which can be used for this purpose, mention should be made of those described in patent FR 2,175,236. Their concentrations in the emulsion depend on the nature of the product to be treated, as well as on the particular aromatic effect that is sought. Concentrations of the order of 10 to 100-200 ppm (parts per million) by weight, based on the weight of flavored tobacco, can generally be used in most practical cases.
L'invention sera illustrée de manière plus détaillée mais non limitative par les exemples qui suivent.The invention will be illustrated in more detail but not limited to by the examples which follow.
Une composition aromatisante de type tabac (origine : Firmenich SA, Genève : Tabac 52.644) a été incorporée à raison de 1% en poids dans une émulsion obtenue en mélangeant les ingrédients suivants (parties en poids) :
- 1) un mélange 10:90 de maltodextrines (origine : Roquette Frères, Beinheim, France et Grain Processing Corporation, Muscatine, Iowa USA)
- 2) alginate de sodium (origine : Alginate Industries Ltd., Grande-Bretagne).
- 1) a 10:90 mixture of maltodextrins (origin: Roquette Frères, Beinheim, France and Grain Processing Corporation, Muscatine, Iowa USA)
- 2) sodium alginate (origin: Alginate Industries Ltd., Great Britain).
La viscosité de ce mélange est de 72 cps.The viscosity of this mixture is 72 cps.
100 Grammes de l'émulsion aromatique ainsi obtenue a été dispersée par giclement à l'aide d'un gicleur Venturi sur 1000 grammes de tabac coupé (mélange de type "american blend"). Le tabac aromatisé a été ensuite laissé au repos pendant 8 semaines, puis il a été utilisé pour la fabrication de cigarettes (test) dont la fumée a été soumise à l'évaluation de la part d'un groupe d'experts aromaticiens. Par comparaison avec l'arôme de cigarettes aromatisées à l'aide de la même composition aromatisante par giclement d'une solution alcoolique de celle-ci (contrôle) (100g de solution de l'arôme à 1% dans l'alcool éthylique à 95% sur 1000 grammes de tabac), on a observé que les cigarettes "test" développaient un arôme plus marqué et plus harmonieux ; elles développaient également une fumée indirecte (side stream) ayant un arôme plus soutenu.100 grams of the aromatic emulsion thus obtained was dispersed by spraying using a Venturi nozzle on 1000 grams of cut tobacco ("American blend" type mixture). The flavored tobacco was then left to rest for 8 weeks, then it was used for the manufacture of cigarettes (test), the smoke of which was subjected to evaluation by a group of flavor experts. By comparison with the aroma of cigarettes flavored with the same flavoring composition by spraying with an alcoholic solution thereof (control) (100g of 1% aroma solution in 95% ethyl alcohol % of 1000 grams of tobacco), it was observed that the "test" cigarettes developed a more marked and more harmonious aroma; they also developed indirect smoke (side stream) with a more sustained aroma.
Une composition aromatisante de type Tabac de Virginie (origine : Firmenich SA, Genève : Tabac 53.476) a été incorporée à raison de 0,5% en poids à l'émulsion décrite à l'Exemple 1.A flavoring composition of Virginia tabac type (origin: Firmenich SA, Geneva: Tabac 53.476) was incorporated at a rate of 0.5% by weight into the emulsion described in Example 1.
100 Grammes de l'émulsion aromatique obtenue à été dispersée par giclement selon la méthode décrite à l'exemple précédent. On a procédé à la fabrication de cigarettes "test" et "contrôle", ainsi qu'à l'évaluation de leur fumée, comme indiqué dans ledit exemple.100 grams of the aromatic emulsion obtained was dispersed by spraying according to the method described in the previous example. The manufacture of "test" and "control" cigarettes, as well as the evaluation of their smoke, as indicated in said example.
Le panel d'experts a pu déterminer que l'arôme développé par les cigarettes "test" possédaient une note plus riche, tandis que le caractère âcre et irritant propre au tabac était amoindri.The panel of experts was able to determine that the aroma developed by the "test" cigarettes had a richer note, while the acrid and irritant character specific to tobacco was lessened.
Une composition aromatisante de type fruité pour tabac (origine : Firmenich SA, Genève : Tabac 53.911) particulièrement adaptée à l'aromatisation de tabac (mélange de tabac de type "flue-" et "air-cured" avec des tabacs orientaux) pour la manufacture de kreteks (cigarettes de type Indonésien) a été incorporée à raison de 1% en poids dans l'émulsion décrite à l'Exemple 1. La fabrication des cigarettes "test" et "contrôle" ainsi que l'évaluation de leur fumée ont été effectuées comme décrit précédemment.A flavoring composition of the fruity type for tobacco (origin: Firmenich SA, Geneva: Tobacco 53.911) particularly suitable for flavoring tobacco (mixture of "flue-" and "air-cured" type tobacco with oriental tobacco) manufacture of kreteks (Indonesian type cigarettes) was incorporated at a rate of 1% by weight in the emulsion described in Example 1. The manufacture of “test” and “control” cigarettes as well as the evaluation of their smoke been performed as described above.
Les cigarettes test développaient un caractère fruité marqué de type banane mûre, avec une tonalité légère de fruit sec.The test cigarettes developed a marked fruity character of ripe banana, with a light hint of dry fruit.
La composition aromatisante utilisée à l'exemple précédent (Tabac 53.911, Firmenich SA) a été incorporée à raison de 1% en poids à l'émulsion obtenue en mélangeant les ingrédients suivants (parties en poids) :
- 1) mélange 10:90 de maltodextrines (origine : Roquette Frères, Beinheim, France et Grain Processing Corporation, Muscatine, Iowa USA)
- 2) alginate de sodium (origine : Alginate Industries Ltd., Grande-Bretagne).
- 3) hydrolysate de collagène (origine : Friedrich Naumann, Memmingen, RFA).
- 1) 10:90 mixture of maltodextrins (origin: Roquette Frères, Beinheim, France and Grain Processing Corporation, Muscatine, Iowa USA)
- 2) sodium alginate (origin: Alginate Industries Ltd., Great Britain).
- 3) collagen hydrolysate (origin: Friedrich Naumann, Memmingen, RFA).
On a ensuite préparé des cigarettes "test" et "contrôle" comme indiqué à l'Exemple 1. L'évaluation de la part d'un groupe d'experts a indiqué que la fumée des cigarettes "test" possédaient un caractère de fruit sec et une note légèrement caramel."Test" and "control" cigarettes were then prepared as shown in Example 1. The evaluation by an expert group indicated that the smoke from the "test" cigarettes had a dry fruit character. and a slightly caramel note.
La composition aromatisante utilisée à l'Exemple 3 (Tabac 53.911, Firmenich SA) a été incorporée à raison de 1% en poids dans l'émulsion obtenue en mélangeant les ingrédients suivants (parties en poids) :
- 1), 2) et 5) voir Exemple 4
- 3) Amidon modifié de maïs (origine : National Starch and Chemical Corp., Bridgewater N.J., USA)
- 4) Laurate de sorbitol (origine : Atlas Chemical Industries N.V., Everberg, Belgique).
- 1), 2) and 5) see Example 4
- 3) Modified corn starch (origin: National Starch and Chemical Corp., Bridgewater NJ, USA)
- 4) Sorbitol Laurate (origin: Atlas Chemical Industries NV, Everberg, Belgium).
En suivant la méthode décrite à l'Exemple 1, on a préparé des cigarettes "test" et "contrôle" qui ont été ensuite soumises à évaluation (voir exemples précédents). Le groupe d'experts a indiqué que la fumée des cigarettes "test" possédaient un caractère de fruit sec et un arôme typique de banane mûre. L'arôme développé par les cigarettes de "contrôle", aromatisées à l'aide d'une solution alcoolique de l'arôme dans l'alcool à 95%, possédait par contre un caractère légèrement gras, beurré et caramel. La fumée développée par les cigarettes "test" était en outre moins irritante grâce à sa note de fond plus fruitée.Following the method described in Example 1, "test" and "control" cigarettes were prepared which were then subjected to evaluation (see previous examples). The expert group reported that smoke from "test" cigarettes had a dry fruit character and a typical aroma of ripe banana. The aroma developed by the "control" cigarettes, flavored with an alcoholic solution of the aroma in 95% alcohol, had on the other hand a slightly fatty, buttered and caramel character. The smoke developed by the "test" cigarettes was also less irritating thanks to its more fruity base note.
Une composition aromatisante pour cigarettes de type "kretek", constituée pour l'essentiel par de l'eugénol a été ajoutée, à raison de 8% en poids, à une émulsion préparée selon la méthode indiquée à l'Exemple 5. On procède à l'aromatisation d'un mélange de tabac, comme indiqué à l'Exemple 1, et conduit ensuite l'évaluation organoleptique sur les cigarettes obtenues par comparaison avec des cigarettes de "contrôle" aromatisées par giclement sur le même type de tabac d'une solution alcoolique (alcool éthylique à 95%) du même arôme.A flavoring composition for “kretek” type cigarettes, consisting essentially of eugenol, was added, at a rate of 8% by weight, to an emulsion prepared according to the method indicated in Example 5. the flavoring of a tobacco mixture, as indicated in Example 1, and then conducts the organoleptic evaluation on the cigarettes obtained by comparison with “control” cigarettes flavored by spraying on the same type of tobacco of a alcoholic solution (95% ethyl alcohol) with the same aroma.
Les cigarettes "test" développaient une fumée dont l'arôme était plus complet tout en possédant un meilleur pouvoir de diffusion.The "test" cigarettes developed a smoke whose aroma was more complete while having a better power of diffusion.
L'évaluation organoleptique répétée après 20 semaines n'a pas indiqué des différences notables de goût.Organoleptic evaluation repeated after 20 weeks did not indicate any significant differences in taste.
Une solution à 20% en poids de menthol dans un mélange 1:1 d'éthanol/propylène glycol a été incorporé à l'émulsion décrite à l'Exemple 5 à raison de 25 parties de solution mentholée pour 100 parties d'émulsion. En suivant la méthode décrite à l'Exemple 1, on a ensuite procédé à l'aromatisation d'un mélange de tabac de type "american blend", en utilisant 100 g d'émulsion aromatisante pour 1 kg de tabac.A 20% by weight solution of menthol in a 1: 1 mixture of ethanol / propylene glycol was incorporated into the emulsion described in Example 5 in an amount of 25 parts of menthol solution per 100 parts of emulsion. Following the method described in Example 1, an American blend of tobacco was then flavored, using 100 g of flavoring emulsion per 1 kg of tobacco.
Le tabac aromatisé a été ensuite laissé au repos pendant 8 semaines, puis il a servi à la fabrication de cigarettes "test" dont la fumée a été soumise à évaluation organoleptique par comparaison avec celle développée par des cigarettes de "contrôle" obtenues par aromatisation à l'aide d'une solution alcoolique du même arôme dans l'alcool à 95%.The flavored tobacco was then left to stand for 8 weeks, then it was used to manufacture "test" cigarettes, the smoke of which was subjected to organoleptic evaluation by comparison with that developed by "control" cigarettes obtained by flavoring. using an alcoholic solution of the same aroma in 95% alcohol.
L'arôme des cigarettes "test" a été trouvé plus marqué que celui des cigarettes de "contrôle".The aroma of "test" cigarettes was found to be more marked than that of "control" cigarettes.
Une évaluation organoleptique a été répétée après 20 semaines et dans ce cas également, le groupe d'experts a indiqué une préférence nette en faveur des cigarettes "test".An organoleptic evaluation was repeated after 20 weeks and in this case too, the group of experts indicated a clear preference in favor of "test" cigarettes.
On a procédé comme indiqué à l'exemple précédent mais en utilisant une émulsion obtenue en mélangeant les ingrédients suivants (parties en poids) :
L'arôme des cigarettes "test" est tout à fait comparable à celui obtenu par l'utilisation de l'émulsion selon l'Exemple 5.
The flavor of the “test” cigarettes is entirely comparable to that obtained by the use of the emulsion according to Example 5.
Dans les exemples décrits plus haut, l'émulsion a été préparée ainsi: Dans un récipient approprié, l'eau a été mise en agitation lente au moyen d'un agitateur magnétique ou d'un agitateur à hélice. Les composants solides constitués par le support hydrosoluble (tel l'amidon, les dextrines ou l'alginate) a été ajouté lentement par petites portions. On laisse ensuite gonfler et dissoudre le support à température ambiante, après quoi l'émulsifiant d'abord et l'arôme ensuite ont été ajoutés à la solution aqueuse maintenue sous agitation jusqu'à l'obtention d'une émulsion homogène et fine.In the examples described above, the emulsion was prepared as follows: In a suitable container, the water was stirred slowly using a magnetic stirrer or a propeller stirrer. The solid components formed by the water-soluble support (such as starch, dextrins or alginate) were added slowly in small portions. The medium is then left to swell and dissolve at room temperature, after which the emulsifier first and the aroma then have been added to the aqueous solution kept stirring until a homogeneous and fine emulsion is obtained.
Claims (6)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CH438/86 | 1986-02-05 | ||
CH43886 | 1986-02-05 |
Publications (3)
Publication Number | Publication Date |
---|---|
EP0235539A2 true EP0235539A2 (en) | 1987-09-09 |
EP0235539A3 EP0235539A3 (en) | 1989-09-27 |
EP0235539B1 EP0235539B1 (en) | 1992-04-29 |
Family
ID=4187034
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP87100873A Expired - Lifetime EP0235539B1 (en) | 1986-02-05 | 1987-01-22 | Process for flavouring tabacco |
Country Status (3)
Country | Link |
---|---|
US (1) | US4785833A (en) |
EP (1) | EP0235539B1 (en) |
DE (1) | DE3778568D1 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0284790A2 (en) * | 1987-03-26 | 1988-10-05 | Firmenich Sa | Aromatized food composition or spice |
EP0366835A1 (en) * | 1988-10-31 | 1990-05-09 | Naarden International N.V. | Process for improving the tast and aroma of tobacco |
Families Citing this family (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP3681410B2 (en) * | 1992-04-09 | 2005-08-10 | フィリップ・モーリス・プロダクツ・インコーポレイテッド | Reconstituted tobacco sheet and method for producing and using the same |
GR1001437B (en) * | 1992-11-05 | 1993-12-30 | Aggelos Kontos | Pastry system for the administration of pharmacologically active substances. |
DE19524197C2 (en) * | 1995-07-03 | 1997-09-04 | Johann Fertl | Process for making cigarettes |
US7032601B2 (en) * | 2001-09-28 | 2006-04-25 | U.S. Smokeless Tobacco Company | Encapsulated materials |
US20040163659A1 (en) * | 2003-02-20 | 2004-08-26 | Sherron James L. | Tobacco flavor applicator |
GB0328644D0 (en) * | 2003-12-11 | 2004-01-14 | Souza Cruz Sa | Smoking article |
US8157918B2 (en) | 2005-09-30 | 2012-04-17 | Philip Morris Usa Inc. | Menthol cigarette |
JP2008125498A (en) * | 2006-11-27 | 2008-06-05 | Tetsuro Asao | Method for producing tobacco leaf |
CN102488323A (en) * | 2011-12-13 | 2012-06-13 | 云南瑞升烟草技术(集团)有限公司 | Tobacco absolute emulsification preparation and application thereof to tobacco leaves |
WO2015097189A1 (en) * | 2013-12-24 | 2015-07-02 | Philip Morris Products S.A. | Flavour containing material |
WO2015097187A1 (en) * | 2013-12-24 | 2015-07-02 | Philip Morris Products S.A. | Flavourant containing material |
EP2944204B1 (en) * | 2014-05-12 | 2022-07-20 | Symrise AG | Synthetic clove particles |
CN111838747B (en) * | 2020-07-23 | 2022-07-01 | 广东省金叶科技开发有限公司 | Stripping composition, stripping reagent, application thereof, preparation method of stripping reagent and method for stripping reconstituted tobacco |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1171043A (en) * | 1967-08-15 | 1969-11-19 | Ncr Co | Tobacco Incorporating Encapsulated Flavouring Material. |
FR2475858A1 (en) * | 1980-02-18 | 1981-08-21 | Chinoin Gyogyszer Es Vegyeszet | FLAVORING COMPOSITIONS FOR THE TEA AND PROCESS FOR THE AROMATISATION OF THE |
EP0070719A1 (en) * | 1981-07-21 | 1983-01-26 | Unilever Plc | Encapsulation of volatile liquids |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3280823A (en) * | 1963-10-01 | 1966-10-25 | Philip Morris Inc | Additive-releasing filter for releasing additives into tobacco smoke |
US3603319A (en) * | 1968-12-13 | 1971-09-07 | Philip Morris Inc | Flavor-releasing smoking article and method of making the same |
US3623489A (en) * | 1969-11-18 | 1971-11-30 | Int Flavors & Fragrances Inc | Tobacco smoking article |
DE2202066C2 (en) * | 1971-01-19 | 1982-06-03 | Firmenich S.A., 1211 Genève | Trimethylcyclohexane, hexene and hexadiene derivatives and their use in food and luxury foods, beverages or pharmaceutical preparations |
DE2964970D1 (en) * | 1978-11-03 | 1983-04-07 | Procter & Gamble | Fluidized bed process for making beverage, food or the like |
US4339422A (en) * | 1980-10-16 | 1982-07-13 | Phillips Petroleum Company | Carbon black manufacture |
-
1987
- 1987-01-22 EP EP87100873A patent/EP0235539B1/en not_active Expired - Lifetime
- 1987-01-22 DE DE8787100873T patent/DE3778568D1/en not_active Expired - Lifetime
- 1987-01-28 US US07/007,855 patent/US4785833A/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1171043A (en) * | 1967-08-15 | 1969-11-19 | Ncr Co | Tobacco Incorporating Encapsulated Flavouring Material. |
FR2475858A1 (en) * | 1980-02-18 | 1981-08-21 | Chinoin Gyogyszer Es Vegyeszet | FLAVORING COMPOSITIONS FOR THE TEA AND PROCESS FOR THE AROMATISATION OF THE |
FR2484205A1 (en) * | 1980-02-18 | 1981-12-18 | Chinoin Gyogyszer Es Vegyeszet | AROMATIZING SUSPENSION FOR THE TEA AND PROCESS FOR THE AROMATISATION OF THE |
EP0070719A1 (en) * | 1981-07-21 | 1983-01-26 | Unilever Plc | Encapsulation of volatile liquids |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0284790A2 (en) * | 1987-03-26 | 1988-10-05 | Firmenich Sa | Aromatized food composition or spice |
EP0284790A3 (en) * | 1987-03-26 | 1991-02-27 | Firmenich Sa | Aromatized food composition or spice |
EP0366835A1 (en) * | 1988-10-31 | 1990-05-09 | Naarden International N.V. | Process for improving the tast and aroma of tobacco |
US5103843A (en) * | 1988-10-31 | 1992-04-14 | Naarden International N.V. | Process for improving the taste and aroma of tobacco |
Also Published As
Publication number | Publication date |
---|---|
EP0235539B1 (en) | 1992-04-29 |
US4785833A (en) | 1988-11-22 |
EP0235539A3 (en) | 1989-09-27 |
DE3778568D1 (en) | 1992-06-04 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
EP0235539B1 (en) | Process for flavouring tabacco | |
CA2108563C (en) | Sheet material for smoking product containing an aromatic substance | |
EP0284790B1 (en) | Aromatized food composition or spice | |
AU701651B2 (en) | Comestibles containing stabilized highly odorous flavor component delivery systems | |
CA2697601C (en) | Use of pea maltodextrin and/or of pea glucose syrup for encapsulating hydrophobic compounds | |
FR2484205A1 (en) | AROMATIZING SUSPENSION FOR THE TEA AND PROCESS FOR THE AROMATISATION OF THE | |
EP1455596A1 (en) | Capsule with fast content solubilization and release | |
FR2502904A1 (en) | PROCESS FOR PRODUCING A COMPOSITION FOR THE AROMATISATION OF THE | |
JPH02177880A (en) | Improving method for flavor and smell of tobacco | |
EP1414313B1 (en) | Composite composition containing sensitive substances | |
EP0234284B1 (en) | Food flavoring process | |
FR3140376A1 (en) | GUM FOR CIGARETTE PAPER, CIGARETTE PAPER AND METHOD FOR PRODUCING IT | |
CH618851A5 (en) | Process for the preparation of a particulate flavouring material | |
CH622687A5 (en) | Smokeable substance | |
WO1995003709A1 (en) | Flavouring method | |
FR2652265A1 (en) | PROCESS FOR PREPARING SUSPENSIONS OF WHOLE PLANTS OR PORTIONS OF FRESH OR DRIED PLANTS AND SUSPENSIONS OBTAINED. | |
BE887542A (en) | FLAVORING COMPOSITIONS FOR TEA AND METHOD FOR FLAVORING TEA | |
CH674918A5 (en) | ||
FR2770375A1 (en) | Use of insoluble protein as food additive carrier | |
FR2811203A1 (en) | PROCESS FOR THE MANUFACTURE OF ENCAPSULATED COFFEE FLAVOR USING ONLY INGREDIENTS EXTRACTED FROM COFFEE BEANS | |
JPS5953320B2 (en) | Method for manufacturing solid oily substances | |
WO1991013135A1 (en) | Method for preparing an aromatic water-soluble plant essence having high organoleptic quality and time stability, and uses thereof in miscellaneous beverages and compositions | |
EP0741968A2 (en) | Artificial sap for the conservation of plants | |
BE497246A (en) | ||
FR2697972A1 (en) | Biscuits based on mustard bran and amylaceous prods. - esp. for eating as a complement to wines and spirits |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
AK | Designated contracting states |
Kind code of ref document: A2 Designated state(s): CH DE ES FR GB IT LI |
|
RIN1 | Information on inventor provided before grant (corrected) |
Inventor name: SALVADORI, GUISEPPE Inventor name: UHDE, GERALD Inventor name: HOLZNER, GUENTER |
|
PUAL | Search report despatched |
Free format text: ORIGINAL CODE: 0009013 |
|
AK | Designated contracting states |
Kind code of ref document: A3 Designated state(s): CH DE ES FR GB IT LI |
|
17P | Request for examination filed |
Effective date: 19900323 |
|
17Q | First examination report despatched |
Effective date: 19910307 |
|
GRAA | (expected) grant |
Free format text: ORIGINAL CODE: 0009210 |
|
AK | Designated contracting states |
Kind code of ref document: B1 Designated state(s): CH DE ES FR GB IT LI |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: IT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT;WARNING: LAPSES OF ITALIAN PATENTS WITH EFFECTIVE DATE BEFORE 2007 MAY HAVE OCCURRED AT ANY TIME BEFORE 2007. THE CORRECT EFFECTIVE DATE MAY BE DIFFERENT FROM THE ONE RECORDED. Effective date: 19920429 Ref country code: GB Effective date: 19920429 |
|
REF | Corresponds to: |
Ref document number: 3778568 Country of ref document: DE Date of ref document: 19920604 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: ES Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 19920809 |
|
GBV | Gb: ep patent (uk) treated as always having been void in accordance with gb section 77(7)/1977 [no translation filed] | ||
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: LI Effective date: 19930131 Ref country code: CH Effective date: 19930131 |
|
PLBE | No opposition filed within time limit |
Free format text: ORIGINAL CODE: 0009261 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT |
|
26N | No opposition filed | ||
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: FR Effective date: 19930930 |
|
REG | Reference to a national code |
Ref country code: CH Ref legal event code: PL |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: DE Effective date: 19931001 |
|
REG | Reference to a national code |
Ref country code: FR Ref legal event code: ST |