EP0419261B1 - Méthode et appareil d'introduction dans un conteneur d'une suspension ou solution de produit dans un propulseur sous pression - Google Patents

Méthode et appareil d'introduction dans un conteneur d'une suspension ou solution de produit dans un propulseur sous pression Download PDF

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Publication number
EP0419261B1
EP0419261B1 EP90310306A EP90310306A EP0419261B1 EP 0419261 B1 EP0419261 B1 EP 0419261B1 EP 90310306 A EP90310306 A EP 90310306A EP 90310306 A EP90310306 A EP 90310306A EP 0419261 B1 EP0419261 B1 EP 0419261B1
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EP
European Patent Office
Prior art keywords
propellant
suspension
container
filling head
solution
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.)
Expired - Lifetime
Application number
EP90310306A
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German (de)
English (en)
Other versions
EP0419261A1 (fr
Inventor
Peter Colin Weston C/O Glaxo Group Res.Ltd. Burt
Laurie Koon Hung C/O Glaxo Group Res.Ltd. Kwok
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Glaxo Group Ltd
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Glaxo Group Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Glaxo Group Ltd filed Critical Glaxo Group Ltd
Priority to AT90310306T priority Critical patent/ATE90053T1/de
Publication of EP0419261A1 publication Critical patent/EP0419261A1/fr
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Publication of EP0419261B1 publication Critical patent/EP0419261B1/fr
Anticipated expiration legal-status Critical
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
    • B65B31/00—Packaging articles or materials under special atmospheric or gaseous conditions; Adding propellants to aerosol containers
    • B65B31/003—Adding propellants in fluid form to aerosol containers

Definitions

  • This invention relates to a method and apparatus for introducing into a container a pharmaceutical substance to be dispensed in aerosol form and a propellant therefor.
  • pharmaceutical substances which are to be dispensed in aerosol form are usually suspended in a mixture of at least two propellants, at least one of which has a high enough boiling point to be liquid at room temperature, and at least one of which has a low enough boiling point to be a gas at room temperature.
  • a liquid, or low pressure, propellant, and a gaseous, or high pressure, propellant are referred to below as a liquid, or low pressure, propellant, and a gaseous, or high pressure, propellant respectively.
  • the pharmaceutical material is first suspended in the liquid propellant by a mixing operation.
  • Each aerosol container is then partly filled with this suspension.
  • a quantity of the gaseous propellant is then introduced into each of the containers using either a cold-fill method or a high-pressure method.
  • the filling operation is carried out at a temperature sufficiently below room temperature for the gaseous propellant to be liquid.
  • Each container is then closed by a closure which includes an outlet valve through which the contents of the container can subsequently be dispensed.
  • the closure is applied to the container before the gaseous propellant is introduced, and that propellant is introduced subsequently into each container by forcing it under pressure into the container through the outlet valve, which during this operation acts in effect as an inlet valve.
  • FIGS. 1 and 2 of the accompanying drawings show diagrammatically a typical known apparatus for introducing into a container a pharmaceutical material and a two-component propellant system.
  • FIG. 1 shows the introduction into a container C of a suspension of a pharmaceutical material in a liquid propellant.
  • Vessel 1 contains a bulk supply of this suspension which is pumped by a pump 2, through a non-return valve 3, into a metering cylinder 4 provided with a vent 5. From there, the suspension passes to a filling head 8. In the inoperative condition the suspension passes through the head 8 to a non-return valve 9 and thence back to the vessel. The suspension is thus kept constantly in circulation.
  • the container is positioned below the head 8, and the valves 3 and 9 are closed.
  • the pneumatic cylinder 6 is then operated to force the piston therein downwardly, thus increasing the pressure in the suspension trapped between the valves 3 and 9 to a level sufficiently to open a valve in filling head 8 and to cause suspension to pass from the filling head into the container C.
  • the valves 3 and 9 are then opened and the valve in filling head 8 shut, and when the piston in the cylinder 6 is withdrawn to its original position the cylinder 4 refills from the vessel 1. Movement of the filling nozzle into and out of engagement with each can is effected by a piston and cylinder arrangement 7.
  • the filling head 8 is arranged to operate only when it is in engagement with a container C.
  • the apparatus of Figure 1 introduces into container C a suspension of pharmaceutical material in a liquid propellant, and after an aerosol valve is crimped on the can C the apparatus shown in Figure 2 operates on it to introduce gaseous propellant.
  • the apparatus of Figure 2 is formed of components which are substantially the same in principle as corresponding components of Figure 1, except that there is nothing corresponding to the non-return valve 9 and there is no recycling. Components in Figure 2 are denoted by reference numerals which correspond to those used in Figure 1, with the addition of 10.
  • the vessel 11 contains gaseous propellant only, under sufficient pressure for it to to be a liquid, and contains no pharmaceutical material.
  • a method of introducing into a container a suspension or solution of a pharmaceutical substance in a propellant held under pressure, the suspension or solution being circulated in a line which includes a filling head which method comprises bringing the filling head into communication with the container; introducing a quantity of such suspension or solution into the container through the filling head; introducing a quantity of high pressure propellant without any of the said substance into the filling head while it is still in communication with the container, thereby to flush through any suspension or solution remaining in the filling head; and withdrawing the filling head from the container.
  • an apparatus for introducing into a container a suspension or solution of a pharmaceutical substance in a propellant held under pressure which comprises a line in which the suspension or solution circulates, the line including a filling head adapted to be brought into and out of communication with the container; means for supplying to the filling head along the line a quantity of the said suspension or solution; and means for supplying to the filling head a quantity of high pressure propellant without any of the said substance, the filling head being so arranged that the flow of propellant without any of the said substance flushes out any suspension or solution remaining in the filling head.
  • the invention also provides a filling head for use in introducing into a container a suspension or solution of a pharmaceutical substance in a propellant held under pressure, comprising an outlet adapted to communicate, in use, with the container; first and second inlets each communicating with the said outlet via a common flow path, through which inlets, in use, propellant containing the said substance, and high pressure propellant not containing the said substance, are respectively introduced; and means for selectively closing the first and second inlets so that fluid entering either inlet cannot flow our of the other.
  • the propellant without the suspension or solution is the same propellant as that in which the substance is held.
  • the propellant is 1,1,1,2-tetrafluoroethane (also known as propellant “134a”).
  • the pharmaceutical substance being filled into the container is salbutomol or beclomethasone dipropionate.
  • the apparatus according to the invention shown in Figure 3 comprises, in effect, something resembling a combination of the apparatus of Figures 1 and 2, but with a common filling head of a novel design.
  • the components shown in Figure 3 are denoted by reference numerals which correspond to those shown in Figure 1, but with the addition of 20 or 30.
  • the vessel 21 contains a suspension of a pharmaceutical substance in a high-pressure propellant
  • the vessel 31 contains a supply of the same propellant alone, i.e. without any pharmaceutical substance suspended therein.
  • the vessel 31 here contains the same propellant, a different high pressure propellant can of course be used.
  • vessel 21 might contain a solution of the pharmaceutical substance, instead of a suspension.
  • Figures 4A-4D show in more detail, and on a larger scale, the filling head 28 used in the apparatus of Figure 3.
  • the head comprises a substantially cylindrical body 40, the lower end of which is adapted, in use, to engage over the upper end of an aerosol container C.
  • a tubular member 43 is mounted for slidable movement within the body 40.
  • the tubular member 43 has a wide base portion 44, a narrower body portion 45 and a still narrower neck portion 46.
  • “wide” and “narrow” refer to diameters.
  • the neck portion 46 of the tubular member 43 penetrates the base of an inverted cup 47, the wall of which surrounds the body portion 45. The body portion 45 can thus slide into the cup 47.
  • the base portion 44 of the tubular member abuts an inwardly extending lip 50 of the body 40.
  • An outwardly extending lip 51 of the cup 47 rests on an internal shoulder 52 of the body 40.
  • a tubular pillar 55 is threadedly engaged with the body 40 such that its lower edge engages on the lip 51 of the cup 47.
  • the pillar 55 thus fits around the wall of the cup 47.
  • a ring 56 is screwed into the pillar 55 so that it is mounted above the cup 47.
  • the neck portion 46 of the tubular member 43 just enters into the ring 56.
  • a sliding seal 58 is fitted between the ring 56 and the neck portion 46.
  • Rubber O-ring seals 59, 60 are also provided between the ring 56 and the pillar 55 and in the base portion 44 of the member 43, where the nozzle of the container C fits (see later).
  • the ring 56 defines an upwardly tapering seat 62 for a correspondingly shaped plug 63.
  • the plug 63 is biassed into the seat by a compression spring 64, the upper end of which acts against an inwardly directed lip 65 of the pillar 55.
  • Inlet pipes 72,73 are fitted into the inlets 69,70 respectively, sealed therein by O-ring seals 74,74'.
  • a ball-bearing 75 which can close against either O-ring seal 74,74' to form a valve. As explained below, the ball bearing 75 is either forced against the O-ring 74 to seal the inlet 69 or against the O-ring 74' to seal the inlet 70.
  • the pillar 55 provides a circular seat for a piston (not shown) which acts to press the fitting head down onto the container C.
  • the inlet 69 is connected to the line which carries the suspension from the metering cylinder 24 to the non-return valve 29.
  • the inlet 70 is connected to the outlet of the metering cylinder 34 which contains propellant.
  • suspension S flows along the line from the metering cylinder 24 to the non-return valve 29 without entering the interior of the pillar 55, being prevented from doing so by the ball bearing valve 75, forced against the O-ring 74 by the over-pressure of propellant P in the line from cylinder 34.
  • the valves 23 and 29 are closed and the cylinder 26 operated to cause the piston therein to move downwardly.
  • the next stage in the filling of the container is to pass a quantity of propellant without any pharmaceutical material suspended therein into the head 28, through the interior of the pillar 55 and of the tubular member 43, and thence into the container. This is done by closing the valve 33 and operating the pneumatic cylinder 36. The increase in the pressure of the propellant which this causes is sufficient to move the ball bearing valve 75. Propellant is unable to pass from the now open inlet 70 to the inlet 69 because of the ball bearing valve 75 which is forced against O-ring 74. This position is shown in Figure 4C.
  • Figure 5 shows an alternative embodiment of a filling head 28 to be used in the apparatus of Figure 3.
  • the head shown in Figure 5 comprises a substantially cylindrical body 80, the lower end of which is adapted, in use, to engage over the upper end of an aerosol container (not shown in this figure).
  • a ring 81 is mounted for longitudinal sliding movement within the body 80 and has an inwardly directed flange 82 on which rests the lower end of a tubular member 83.
  • the upper portion of the tubular member 83 is surrounded by an inverted cup 84.
  • the cup 84 is in turn surrounded by the annular lower portion of a pillar 85.
  • the annular portion is screw threaded into the body 80 to retain the cup 84 in place and sealing is provided by an O-ring seals 86 and a sliding seal 87.
  • the tubular member 83 is urged into engagement with the flange 82 by a compression spring 88, the upper end of which bears against a face of the cup 84.
  • the pillar 85 has a pair of opposed inlets 89 and 90.
  • the inlet 89 is connected to the line which carries suspension from the metering cylinder 24 to the non-return valve 29.
  • the inlet 90 is connected to the outlet of the metering cylinder 34 which contains propellant.
  • the inlets 89 and 90 communicate with the interior of the tubular member 83 via respective poppet valves 91 and 92 which are biassed by compression springs 93 and 94 into their closed positions.
  • suspension flows along the line from the metering cylinder 24 to the non-return valve 29 without entering the interior of the tubular member 83, being prevented from doing so by the valve 91.
  • the valves 23 and 29 are closed, and the cylinder 26 operated to cause the piston therein to move downwardly.
  • the increase in pressure in the suspension in the metering cylinder 24 which is caused by this is sufficient to overcome the force of the spring 93 holding the valve 91 shut, and suspension is thus able to flow from the inlet 89, through the interior of the tubular member 83, into the container.
  • the valve 92 remains closed, and indeed the effectiveness of the seal which it provides is increased by the head 95 of the valve 91 engaging the head 96 of the valve 92. Thus, suspension is unable to pass from the inlet 89 to the inlet 90 and contaminate the inlet 90.
  • the next stage in the filling of the container is to pass a quantity of propellant without any pharmaceutical material suspended therein into the head 28, through the tubular member 83, and thence into the container. This is done by closing the valve 33 and operating the pneumatic cylinder 36. The increase in the pressure of the propellant which this causes is sufficient to open the valve 92 to permit propellant through the head 28. Propellant is unable to pass from the inlet 90 to the inlet 89 because of the action of the valve 91.
  • this embodiment also provides that when the head 28 is lifted from the aerosol container after the filling operation has been completed, such material as escapes from the lower end of the head consists substantially entirely of propellant, and no pharmaceutical material escapes.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Vacuum Packaging (AREA)
  • Containers And Packaging Bodies Having A Special Means To Remove Contents (AREA)
  • Medicinal Preparation (AREA)
  • Basic Packing Technique (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Filling Or Discharging Of Gas Storage Vessels (AREA)
  • Diaphragms For Electromechanical Transducers (AREA)
  • Filling Of Jars Or Cans And Processes For Cleaning And Sealing Jars (AREA)
  • Colloid Chemistry (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Claims (12)

  1. Méthode d'introduction dans un conteneur (c) d'une suspension ou d'une solution d'une substance pharmaceutique dans un propulseur sous pression, la suspension ou la solution circulant dans une conduite qui comporte une tête de remplissage (28), laquelle méthode comprend la mise en communication de la tête de remplissage (28) avec le conteneur (c); d'introduction d'une quantité d'une telle suspension ou solution dans le conteneur à travers la tête de remplissage (28); d'introduction d'une quantité de propulseur sous pression sans aucune desdites substances dans la tête de remplissage (28) alors qu'elle est encore en communication avec le conteneur (c), pour évacuer ainsi toute suspension ou solution restant dans la tête de remplissage (28); et le détachement de la tête de remplissage (28) du conteneur (c).
  2. Méthode selon la revendication 1, dans laquelle le propulseur qui contient ladite substance et ledit propulseur sans aucune desdites substances sont les mêmes.
  3. Méthode selon la revendication 1 ou 2, dans lequel le propulseur est du 1,1,1,2-tétrafluoroéthane.
  4. Méthode selon l'une quelconque des revendications précédentes, dans laquelle la substance est du salbutamol
  5. Méthode selon l'une quelconque des revendications 1 à 3, dans laquelle la substance est du dipropionate de beclométhasone.
  6. Appareil pour introduire dans un conteneur (c) une suspension ou une solution d'une substance pharmaceutique dans un propulseur sous pression, qui comprend une conduite dans laquelle circule la suspension ou la solution, la ligne comportant une tête de remplissage (28) adaptée pour être mise en et hors communication avec le conteneur (c); un moyen (21, 22, 23, 24) pour fournir à la tête de remplissage (28) par la conduite, une quantité de ladite suspension ou solution, et un moyen (31, 32, 33, 34) pour fournir à la tête de remplissage (28) une quantité de propulseur sous haute pression sans aucune desdites substances, la tête de remplissage (28) étant agencée de telle sorte que le flux de propulseur sans aucune desdites substances évacue toute suspension ou solution restant dans la tête de remplissage (28).
  7. Appareil selon la revendication 6, dans lequel la tête de remplissage (28) comprend un passage pour la suspension ou la solution et pour le propulseur seul, une entrée (70) pour la suspension ou solution et une entrée (69) pour le propulseur seul, chaque entrée (69, 70) communiquant avec ledit passage, et une pièce formant valve (75) mobile entre une position fermant l'entrée (70) pour la suspension ou la solution et une position fermant l'entrée (69) pour le propulseur seul, à tout moment une seule desdites entrées (69, 70) est ainsi en communication avec ledit passage.
  8. Appareil selon la revendication 7, dans lequel la pièce formant valve est une pièce sphérique (75).
  9. Appareil selon la revendication 6, dans lequel la tête de remplissage (28) comprend un passage pour la suspension ou la solution et pour le propulseur seul, une entrée (70) pour la suspension ou la solution et une entrée (69) pour le propulseur seul, chaque entrée (69, 70) communiquant avec ledit passage, et une pièce formant valve (95, 96) dans chaque entrée, les entrées (69, 70) étant opposées l'une à l'autre et les pièces formant valve (95, 96) étant agencées de sorte que lorsque l'une est ouverte elle appuie davantage l'autre dans sa position fermée.
  10. Tête de remplissage à utiliser pour l'introduction dans un conteneur (c) d'une suspension ou d'une solution d'une substance pharmaceutique dans un propulseur sous pression, comprenant une sortie adaptée pour communiquer, lors de l'utilisation avec le conteneur (c); des première (69) et seconde (70) entrées communiquant avec ladite sortie via un chemin de flux commun, à travers lesquels entrées (69, 70) on introduit, lors de l'utilisation, respectivement un propulseur contenant ladite substance, et un propulseur sous haute pression ne contenant pas ladite substance; et un moyen (75; 95, 96) pour fermer sélectivement les première et seconde entrées (69, 70) afin que le fluide entrant par m'importe quelle entrée ne puisse s'écouler par l'autre.
  11. Tête de remplissage selon la revendication 10, comprenant une pièce formant valve (75) fermant alternativement les première et seconde entrées, la pièce formant valve étant une pièce sphérique.
  12. Tête de remplissage selon la revendication 10, comprenant une pièce formant valve (95, 96) dans chacune des première et seconde entrées (69, 70), les entrées étant opposées l'une à l'autre et la pièce formant valve étant agencée de telle sorte que lorsque l'une est ouverte elle appuie davantage l'autre dans sa position fermée.
EP90310306A 1989-09-21 1990-09-20 Méthode et appareil d'introduction dans un conteneur d'une suspension ou solution de produit dans un propulseur sous pression Expired - Lifetime EP0419261B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT90310306T ATE90053T1 (de) 1989-09-21 1990-09-20 Verfahren und vorrichtung zum einfuehren eines in einem treibmittel unter druck suspendierten oder geloesten produkts in einen behaelter.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB898921337A GB8921337D0 (en) 1989-09-21 1989-09-21 Method and apparatus
GB8921337 1989-09-21

Publications (2)

Publication Number Publication Date
EP0419261A1 EP0419261A1 (fr) 1991-03-27
EP0419261B1 true EP0419261B1 (fr) 1993-06-02

Family

ID=10663409

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Application Number Title Priority Date Filing Date
EP90310306A Expired - Lifetime EP0419261B1 (fr) 1989-09-21 1990-09-20 Méthode et appareil d'introduction dans un conteneur d'une suspension ou solution de produit dans un propulseur sous pression

Country Status (14)

Country Link
EP (1) EP0419261B1 (fr)
JP (1) JP2809852B2 (fr)
AT (1) ATE90053T1 (fr)
AU (1) AU634817B2 (fr)
CA (1) CA2025779C (fr)
DE (1) DE69001793T2 (fr)
DK (1) DK0419261T3 (fr)
ES (1) ES2043290T3 (fr)
FI (1) FI92171C (fr)
GB (2) GB8921337D0 (fr)
HK (1) HK82397A (fr)
IE (1) IE63939B1 (fr)
NZ (1) NZ235401A (fr)
ZA (1) ZA907534B (fr)

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FR2669616B1 (fr) * 1990-11-23 1993-01-08 Atochem Procede de remplissage de futs par des liquides non miscibles et ses applications, notamment a l'enfutage du phosphore blanc.
IT1253976B (it) * 1992-04-01 1995-09-05 Bombole con aerosol ad aria compressa, di tipo perfezionato ed apparecchio per la loro ricarica.
CH682654A5 (de) * 1992-05-18 1993-10-29 Birchmeier & Cie Ag Aerosoldose.
GB9306292D0 (en) * 1993-03-26 1993-05-19 Glaxo Group Ltd Method
DE9422052U1 (de) * 1994-01-04 1997-10-30 Adolf Würth GmbH & Co. KG, 74653 Künzelsau Befüllgerät zum Befüllen eines wiederbefüllbaren Ausgabebehälters und wiederbefüllbarer Ausgabebehälter
DE4429161A1 (de) * 1994-01-04 1995-07-06 Adolf Wuerth Gmbh & Co Kg Wiederbefüllbarer Ausgabebehälter, Befüllgerät und Verfahren zum Befüllen des Ausgabebehälters
AU713700B2 (en) * 1994-01-04 1999-12-09 Adolf Wurth Gmbh & Co. Kg A filling device for a refillable distributing container
DE4423916C2 (de) * 1994-07-07 1996-05-30 Boehringer Ingelheim Kg Verfahren zur Druckabfüllung
DE19513886A1 (de) * 1995-04-19 1996-10-24 Willi Georg Pfeiffer Wiederbefüllbare Aerosoldose
DE19717080C2 (de) * 1996-12-19 2001-12-06 Manfred Stadler Wiederholt nachfüllbare Spraydose oder -flasche
DE29713077U1 (de) * 1997-07-23 1998-11-26 Adolf Würth GmbH & Co. KG, 74653 Künzelsau Ventileinheit zur Befüllung von Aerosol-Dosen
SE9801399D0 (sv) 1998-04-21 1998-04-21 Astra Pharma Prod Method and apparatus for filling containers
SE9801398D0 (sv) 1998-04-21 1998-04-21 Astra Pharma Prod Method and apparatus for filling containers?
DE20103988U1 (de) * 2001-03-07 2001-07-12 Seaquist Perfect Dispensing GmbH, 44319 Dortmund Abfüllkopf zur Befüllung von Behältern mit einem fluidförmigen Medium
US8448677B2 (en) * 2009-06-09 2013-05-28 Surface Technologies Ip Ag Apparatus and method for refilling a refillable container
CN102470938B (zh) * 2009-12-09 2013-06-05 东洋喷雾工业株式会社 喷射剂的填充装置
DE102013206543A1 (de) * 2012-07-16 2014-01-16 Robert Bosch Gmbh Vorrichtung zum Befüllen von Behältnissen
CN103879944B (zh) * 2012-12-19 2016-04-20 昆山晶科微电子材料有限公司 氢氟酸灌装系统
CN108349598A (zh) * 2015-12-14 2018-07-31 Khs科波普拉斯特有限责任公司 用于通过在压力下导入到预制坯件中的填充物由预制坯件制造填充有液态填充物的容器的方法和装置
CN109095419B (zh) * 2018-06-21 2021-04-20 上海西西艾尔启东日用化学品有限公司 一种二氧化碳气雾剂制造系统和工艺

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US3583446A (en) * 1968-06-24 1971-06-08 Frank E Rush Jr Process and apparatus for loading containers
US3636993A (en) * 1968-12-31 1972-01-25 Ciba Geigy Corp Adapter for filling head for filling aerosol dispenser
US3642035A (en) * 1970-07-17 1972-02-15 Ciba Geigy Corp Device for the filling of dispersers of the aerosol type having a separate self-contained propulsion unit
JPS5323008A (en) * 1976-08-16 1978-03-03 Matsushita Electric Ind Co Ltd C ommutatorless motor
JPS5820486Y2 (ja) * 1978-02-24 1983-04-28 凸版印刷株式会社 充填ノズル
HU189881B (en) * 1984-01-06 1986-04-28 Pamper, Viktor, Hu Method for spreading bulk materials from closed space and apparatus for charging the material or materials to be spread into closed space and for pressurizing same

Also Published As

Publication number Publication date
ZA907534B (en) 1991-06-26
GB9020501D0 (en) 1990-10-31
EP0419261A1 (fr) 1991-03-27
DE69001793T2 (de) 1993-09-16
FI92171B (fi) 1994-06-30
IE63939B1 (en) 1995-06-28
NZ235401A (en) 1993-02-25
CA2025779C (fr) 1999-09-14
AU634817B2 (en) 1993-03-04
ATE90053T1 (de) 1993-06-15
AU6301190A (en) 1991-03-28
DK0419261T3 (da) 1993-10-04
IE903407A1 (en) 1991-04-10
FI92171C (fi) 1994-10-10
HK82397A (en) 1997-06-27
FI904627A0 (fi) 1990-09-20
CA2025779A1 (fr) 1991-03-22
JP2809852B2 (ja) 1998-10-15
JPH03212395A (ja) 1991-09-17
GB2236146A (en) 1991-03-27
GB2236146B (en) 1993-05-12
GB8921337D0 (en) 1989-11-08
ES2043290T3 (es) 1993-12-16
DE69001793D1 (de) 1993-07-08

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