Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
  • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
  • B05B11/00—Single-unit hand-held apparatus in which flow of contents is produced by the muscular force of the operator at the moment of use
  • B05B11/01—Single-unit hand-held apparatus in which flow of contents is produced by the muscular force of the operator at the moment of use characterised by the means producing the flow
  • B05B11/02—Membranes or pistons acting on the contents inside the container, e.g. follower pistons
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
  • A61M11/00—Sprayers or atomisers specially adapted for therapeutic purposes
  • A61M11/006—Sprayers or atomisers specially adapted for therapeutic purposes operated by applying mechanical pressure to the liquid to be sprayed or atomised
  • A61M11/007—Syringe-type or piston-type sprayers or atomisers
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
  • A61M5/00—Devices for bringing media into the body in a subcutaneous, intra-vascular or intramuscular way; Accessories therefor, e.g. filling or cleaning devices, arm-rests
  • A61M5/178—Syringes
  • A61M5/24—Ampoule syringes, i.e. syringes with needle for use in combination with replaceable ampoules or carpules, e.g. automatic
  • A61M5/2422—Ampoule syringes, i.e. syringes with needle for use in combination with replaceable ampoules or carpules, e.g. automatic using emptying means to expel or eject media, e.g. pistons, deformation of the ampoule, or telescoping of the ampoule
  • A61M5/2429—Ampoule syringes, i.e. syringes with needle for use in combination with replaceable ampoules or carpules, e.g. automatic using emptying means to expel or eject media, e.g. pistons, deformation of the ampoule, or telescoping of the ampoule by telescoping of ampoules or carpules with the syringe body
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
  • A61M5/00—Devices for bringing media into the body in a subcutaneous, intra-vascular or intramuscular way; Accessories therefor, e.g. filling or cleaning devices, arm-rests
  • A61M5/178—Syringes
  • A61M5/24—Ampoule syringes, i.e. syringes with needle for use in combination with replaceable ampoules or carpules, e.g. automatic
  • A61M5/2448—Ampoule syringes, i.e. syringes with needle for use in combination with replaceable ampoules or carpules, e.g. automatic comprising means for injection of two or more media, e.g. by mixing

Definitions

• the present invention relates to a device for packaging liquid or liquid and solid substances, comprising a generally cylindrical elongated ampoule of circular section, with two compartments arranged in the extension of one another, separated by an intermediate plug movable in elastomer, and each containing a different substance, the two substances having to be brought into contact with each other to constitute a liquid mixture for medical or paramedical use, this device being designed firstly to ensure during a first period of time, storage conditions for each of these substances, secondly to allow, during a second time interval, their contact, and thirdly to allow, during a third time interval, the use of this liquid mixture discharged out of the packaging device, in which the ampoule is closed at one of its ends, open te at its other end and comprises at least one cylindrical zone of narrowed circular section to define a retré ⁇ catorium inside this bulb and at least one cylin ⁇ dric zone of wide circular section; in which, during the first time interval corresponding to the storage phase, said cylindrical zone of narrowe
• US Patent No. 3,563,415 describes a liquid dispenser of the drip type, comprising a bottle with two compartments, one of which contains a powder and the other a liquid solvent, the two substances being intended to be mixed to constitute a medicament liquid. These two compartments are separated by an intermediate stopper locked in position in a narrow neck, during the storage phase of the dispenser.
• This neck also contains a shutter composed of a first element capable of sliding inside this neck, provided with a radial channel and with a second element arranged to adapt to the first element to close this radial channel. .
• the compartment containing the powder has a diameter substantially larger than that of the neck. At the time of use, the obturator is inserted into the cervix.
• This device is not suitable for use as an injection syringe or as a sprayer.
• the only intended use is for use as a two-compartment packaging device, the liquid medicament resulting from the mixture of the two components flowing by gravity out of the bottle.
• the European patent application published under No. 0 144 483 describes a syringe of the mixing syringe type, comprising a syringe body divided, during the storage phase, into two compartments by an intermediate stopper.
• the body of this syringe has a substantially cylindrical shape and its distal end carries a needle while its posterior end is closed off by the head of a piston.
• the body of the syringe comprises, substantially in its middle, a lateral deformation, for example a convex bulge, defining a bypass trajectory allowing the transfer of a liquid contained in the posterior compartment to the anterior compartment or chamber mixture, when the intermediate plug is pushed up to the height of this deformation.
• the original substance to be lyophilized which is usually in liquid form, is in fact contained in a compartment delimited on the one hand by the walls inside from the body of the syringe and on the other hand by a surface of the intermediate plug.
• the distal of the syringe remains open end while its other end is to be closed so the sealed by the intermediate grumpy. This sealing is difficult to achieve during the freeze-drying phase which is accompanied, in known manner, by freezing during which the elastomer sealing plug loses all or part of these elasticity properties.
• means must be provided for closing the distal end of the syringe equipped with a needle which opens directly into the anterior compartment initially containing the lyophilisate and serving as a mixing chamber.
• the present invention proposes to overcome the drawbacks of the known systems described above by proposing a packaging device with two compartments allowing the mixing of two substances respectively contained in the two compartments, and to use this mixture as a substance for injection by means of a syringe, substance to be sprayed by means of a sprayer or substance to be driped or by and.
• Another advantage of the device is that all the filling and positioning operations for the various elements can be carried out automatically in very large series, the bulbs traveling side by side without any intermediate support on conveyor belts or trays intended for bring them to different filling and / or assembly stations.
• the packaging device characterized in that the movable intermediate plug has, in the relaxed state in the cylindrical zone of wide circular section, a shape different from the circular shape, a lower surface on the surface of "the cross section of said area of wide circular section, and at least one transverse dimension equal to the diameter of said area of wide circular section, and in that the movable intermediate plug has, in the compressed state in the cylindrical zone of narrowed circular section, a circular shape whose diameter is equal to that of the cross section of this zone.
• the bulb comprises a single cylindrical zone of narrowed circular section formed on the side of its open end and a single cylindrical zone of wide circular section formed on the side of its closed end, this cylindrical zone of narrowed circular section essentially comprising said second compartment and this cylindrical zone of wide circular section essentially comprising said first compartment.
• the bulb comprises a single cylindrical area of narrowed circular section formed between a first cylindrical area of wide circular section and a second cylindrical area of wide circular section, said cylindrical area of narrowed circular section essentially comprising said second compartment and the second cylindrical zone of wide circular section essentially comprising said first compartment.
• said cylindrical zone of narrowed circular section may comprise three sectors, the first of which has a diameter adapted to ensure a tight blocking of the piston-valve during the storage phase, the second of which defines said second compartment and the last of which has a diameter adapted to ensure an etan ⁇ blocking of the movable intermediate plug during this same sto ⁇ ckage phase.
• the bulb comprises a first cylindrical area of wide circular section, a first cylindrical area of narrowed circular section, a second cylindrical area of wide circular section, a second cylindrical area of narrowed circular section and a third cylindrical zone of wide circular section, the first cylindrical zone of narrowed circular section having a diameter suitable for ensuring a tight blocking of the piston-valve during the storage phase and the second cylindrical zone of narrowed circular section having a diameter suitable for ensuring a tight locking of the movable intermediate plug during this same phase, the cylindrical zones of wide circular section respectively defining said second and said first compartment.
• the first cylindrical zone of narrowed circular section has a divergent conicity in the direction of the open end of the bulb.
• the movable intermediate plug advantageously has a shape general cylindrical and its lateral surface has an at least approximately polygonal section in the relaxed state.
• the movable intermediate plug has a generally cylindrical shape and its lateral surface has an approximately oval section in the relaxed state.
• the obtu ⁇ ration member which can have a generally cylindrical shape and its lateral surface can have an at least approximately polygonal shape in the relaxed state or an at least approximately oval shape in this same state.
• the movable intermediate plug may have a notch formed over part of its height, this notch opening into the surface disposed. opposite the bottom of the bulb.
• FIG. 1 represents a view in axial section of the packaging device according to the invention in its storage position
• FIG. 2 represents a first phase of filling the ampoule
• FIG. 3A is a view in axial section illustrating a second phase of manufacturing the device, in particular when one of the conditioned substances is lyophilized
• Figures 3B and 3C are plan views, from above of the bulb as shown in FIG. 3A,
• FIG. 4 represents a subsequent phase of filling the ampoule, at the end of the lyophilization of one of the substances which it contains
• FIG. 5 represents the phase of fitting the movable intermediate plug after filling the first compartment of the bulb
• FIG. 6 illustrates the filling phase of the second compartment of the bulb
• FIG. 7 illustrates the positioning of the injector
• FIG. 8 is a partial longitudinal section view illustrating the phase of use of the packaging device after mixing the two substances respectively contained in the two compartments of the ampoule
• FIG. 9 illustrates the packaging device used as an injection syringe
• FIG. 10 illustrates the packaging device used as a sprayer
• FIG. 11 represents a view in axial section of another embodiment of the ampoule of the packaging device according to the invention.
• FIG. 12 ' represents a view in axial section of a variant of the bulb of the conditioning device illustrated by FIGS. 1 to 10.
• the packaging device with two compartments of substances for medical or paramedical use essentially comprises a bulb 10 of generally cylindrical shape, an injector 11 associated with this bulb, a bulb cover 12 coupled to the injector 11 and re ⁇ covering substantially the entire bulb and a tip cover 13, also coupled to the injector 11, intended to protect a tip 14 secured to one end of the injector 11.
• the injection nozzle can carry a needle 9 as shown more especially fig. 9 and the packaging device then becomes a pre-filled mixing syringe or a spray nozzle 8 as shown more particularly in FIG. 10, and the packaging device then becomes a nasal sprayer or a dropper device or a pouring spout, etc.
• the injector 11 comprises a capsule 15 comprising a cylindrical sleeve which is closed at one end by a bottom secured to the needle-holder tip 14 and open at its opposite end in which the open end of the bulb is enclosed. 10.
• This open end of the capsule 15 carries two fins 16 used in a manner known per se at the time of injection.
• the injector also includes a piston-valve 1? mounted inside the capsule 15 and fixed to its bottom, for example by microwave welding.
• This piston-valve consists of a piston rod 18 carrying a closure member 19 which plays the role of piston head in certain phases of use which will be described in more detail below.
• the bulb 10 closed at one of its ends comprises, on the side of its open end, a first cylindrical zone of wide circular cross section 20 followed by a cylindrical zone 21 of circular cross section connected to the preceding zone 20 by a first zone of frustoconical connection 22.
• the cylindrical zone of circular cross section 21 is followed by a second cylindrical zone of wide circular section 23 connected to the previous one by a second frustoconical connection zone 24.
• a movable intermediate plug 25 is partially engaged in the cylindrical zone of narrowed circular section, on the side of the second frustoconical connection zone 24.
• the shutter member 19 of the piston-valve 17 is partially engaged in this zone cylindrical with a narrowed circular section 21 on the side of the first frustoconical connection zone 22.
• the movable intermediate plug 25 delimits with the bottom of the bulb a first compartment 26 subsequently called the mixing chamber, containing in storage a lyophilisate 27 or any other substance intended to be mixed with another sub- stance 28, for example a liquid solvent which is contained during storage in a second compartment 29 disposed between the movable intermediate plug 25 and the closure member 19.
• the two compartments are sealed the movable intermediate plug 25 and the substances which they contain are isolated from one another.
• FIGS. 2 to 8 will make it possible to understand the different phases of filling and assembly which result in the condi ⁇ tion device with two compartments as shown in its storage position in FIG. 1.
• the ampoule 10 is firstly filled with a liquid substance 27 'which, after a lyophilization operation known per se, will transform into a lyophilisate 27 contained in the mixing chamber 26 of the bulb.
• the cylindrical region of circular section re * trécie 21 advantageously comprises three sectors 21a, 21b and 21c.
• the sector 21a is called the sealed storage sector of the shutter member 19. Its diameter is defined in such a way that it ensures a tight blocking of said shutter member 19 during the storage phase of the packaging device.
• 21c sector is called waterproof storage area of the movable intermediate stopper 25.
• the central sector 21b is an intermediate sector between the two storage sectors. Its diameter can be equal to that of the two storage sectors 21a and 21c, but this condition is not essential. The only necessary condition is that the piston-valve remains sealed during its entire phase of movement through the cylindrical region of narrowed circular section, that is to say through the three sectors 21a, 21b and 21c.
• the diameter of the intermediate sector 21b may be somewhat larger than that of the sectors 21a and 21c, so that the tightening exerted on the shutter member 19 is reduced in this sector, but this diameter may in no case exceed a limit from which the piston-valve loses its tightness.
• the movable intermediate plug 25 is partially engaged in the second tronconi ⁇ connection zone 24 during the storage phase. In this zone, the corresponding part of this plug is less compressed than the part which is engaged in the cylindrical zone of narrowed circular section 21, and will be able to return very quickly to its initial shape as soon as the movable intermediate plug 25 will be pushed into the cylindrical zone of wide circular section.
• FIG. 3A illustrates the prepositioning of the movable intermediate plug 25 for the lyophilization phase.
• Fig. 3B shows a plan view of the movable intermediate plug 25 in place in the first cylindrical zone of wide circular section 20.
• FIG. 3C shows the plug in place in the cylindrical zone of narrowed circular section 21 of the bulb 10.
• This plug is made of an elastomeric material and is therefore deformable when subjected to stress. In the relaxed state, its section is polygonal, for example square, so that 30 days appear between the side wall of the stopper and the inner wall of the chamber. hen, when said plug is engaged in the first cylindrical zone of wide circular section 20 of the bulb 10.
• the shape of the movable intermediate plug is not however limited to a polygonal shape.
• the "mobile intermediate erouchon may comprise a notch or a recess 25a * intended to facilitate the evacuation of the vapors, according to arrow A ', during lyophilization.
• the movable intermediate plug 25 is pressed into the bulb 10 to a depth sufficient for its anterior end to penetrate the first zone of frustoconical connection 22 and seals this hen hermetically.
• This first insertion of the mobile intermediate plug is obtained by means of an upward thrust exerted on the body of the bulb, the mobile intermediate plug 25 being in abutment against the upper wall 31 of the freeze-drying enclosure or by means of a push downward exerted by this upper wall 31, or a movable plate disposed inside the lyophilisa ⁇ tion enclosure.
• Means can be provided to create a partial vacuum inside the freeze-drying enclosure at the end of this operation so that this vacuum also prevails inside the bulb 10. From the moment when the movable intermediate plug 25 is pressed into the neck of the bulb and ensures a tight closure of the latter, the partial vacuum will remain inside this bulb, that is to say above the lyophilisate 27. This condition is however not required and a controlled atmosphere can overcome the lyophilisate, this atmosphere being by example consisting of neutral gas.
• the intermediate plug 25 is brought, possibly by mechanical means schematically represented by the arrow 33, in the vicinity of the lower end of the cylindrical zone of narrowed circular section 21.
• the mechanical means 33 are necessary in certain cases, but superfluous in others.
• the pressure difference can possibly bring about the intermediate plug 25 to slide without external assistance through the intermediate sector 21b to lock in position in the sealed storage sector 21c.
• Fig. 6 illustrates the next phase which consists in introducing into the upper compartment 29 a liquid solvent 28 intended to be mixed with the lyophilisate 27 in order to reconstitute the drug to be injected or to be absorbed, for example by spraying, to a patient.
• the next phase illustrated in fig. 7 consists in mounting the injector 11 on the bulb 10 by engaging the shutter member 19 of the piston-valve 17 in the neck of the bulb Up to the sector 21a of the cylindrical zone of narrowed circular section 21
• the filling of the upper chamber 29 by means of the solvent 28 is carried out in an atmosphere of carbon dioxide, a certain volume of which is initially trapped between the sealing member 19 and the upper surface. of said liquid 28.
• This volume 34 is rapidly dissolved in the liquid solvent 28, which has the consequence of creating a depression which causes an equivalent volume rise in the movable intermediate plug 25.
• This final state is shown in FIG. 1 and corresponds to the storage position of the packaging device.
• the bulb cover 12 is removed, which is replaced by the tip cover 13.
• the latter is dimensioned in such a way that it suffices to press on its flat bottom while holding the syringe by the fins 16 for gradually bringing the bulb into the position shown in FIG. 8.
• This movement causes the displacement of the piston-valve 17 towards the interior of the cylindrical zone of narrowed circular section 21.
• the movable intermediate plug exits from this zone under the pressure fully transmitted by the liquid 28 and enters the zone of entrance to the mixing chamber where it expands, resuming its initial shape shown in fig. 3B, i.e. the form in which 30 Days appear between its lateral surface and the interior walls of the bulb.
• the friction forces of the movable intermediate stopper against the bulb tend to keep this stopper in this position, while the forces generated by the pressure exerted by the intermediary of the liquid would tend to make it advance in the mixing chamber.
• the dimensions of the movable intermediate plug and those of the openings are preferably determined in such a way that the frictional forces are greater than the thrust forces, so that the movable intermediate plug 25 remains in place and the liquid is transferred from the second compartment in the mixing chamber through the 30 days.
• the movable intermediate plug 25 thus remains in position until all the liquid is transferred and Until the shutter member 19 is pressed against its surface superior.
• the liquid solvent 28 dissolves the lyophilisate contained in the mixing chamber 26.
• the solution obtained constitutes the medicament to be injected, sprayed or poured dropwise or in the form of a jet.
• the piston-valve 17 comprises at least one peripheral tongue 35 whose diameter, in the relaxed state, is slightly greater than the diameter of the second cylindrical zone of wide circular section 23 to guarantee that the medicament is discharged through a radial duct 36 formed in the shutter member 19 and connected to an axial duct 37 passing through the piston rod 18 to connect to a needle 9 (see fig. 9), a sprayer 8 (see fig. 10) or any other available ⁇ suitable to release the drug.
• a needle 9 see fig. 9
• a sprayer 8 see fig. 10
• any other available ⁇ suitable to release the drug When the operator pushes the bulb in the direction of the fins of the capsule, the mixture is forced back towards the radial channel through the 30 days.
• the intermediate plug 25 is pushed back to the bottom of the bulb 10 and the shutter member 19 is pressed against the surface of said movable intermediate plug. It is obvious that the shape and dimensions of the movable intermediate plug must be such that it slides axially without tilting inside the bulb.
• a filter 38 can be interposed between a base 39 carrying the piston rod 18 and the bottom of the capsule 15.
• the cylindrical zone of narrowed circular section 21 of the previous example which comprises "three sectors 21a, 21b and 21c which are not very different, can be replaced by three clearly delimited zones.
• This embodiment is illustrated in FIG. 11.
• the bulb 10 ' closed at one of its ends, comprises, on the side of its open end, a first cylindrical zone of wide circular section 20' followed successively by a first cylindrical zone of narrowed circular section 21 ' a, a second cylindrical zone of wide circular section 21 'b, a second cylindrical zone of narrowed circular section 21' c and a third cylindrical zone of wide circular section 23 '.
• the first cylindrical zone of circular narrowed section 21 ′ a corresponds to sector 21a of the zone cylindrical with a narrowed circular section 21 of the bulb 10
• the second cylindrical region with a narrowed circular section 21'c corresponds to sector 21c of the cylindrical area with a narrowed circular section 21 of the bulb 10
• the second cylindrical section section wide circular 21 'b corresponds to the intermediate sector 21b of the cylindrical region of narrowed circular section 21 of the bulb 10.
• the intermediate plug is prepositioned in the secon ⁇ of the cylindrical zone 21 'b of wide circular section during the lyophilization phase, which allows the evacuation of the vapors through the Days due to the elastic deformation of this plug, as previously described.
• the shut-off member of the piston-valve is positioned in the first cylindrical zone of narrowed circular section 21 ′ a and the intermediate plug is in place in the second cylindrical zone of circular narrowed section 2Pc .
• the diameters from cylindrical zones Se wide circular section 21 ′ b and 23 ′ are such that the piston-valve, and more particularly the annular tongue or tongues arranged under the radial channel, fulfill their role as “piston rings” or “scrapers” ", in elastic support against the interior walls of the bulb, and prevent any leakage of liquid to be injected.
• the intermediate plug is made of elastomer and has a polygonal, elliptical, regular or irregular, symmetrical or asymmetrical shape which has days or openings when it is in place in a cylindrical area of wide circular section. and ensures perfect sealing when it is in place in a cylindrical zone of narrowed circular section.
• it could also include a central slot or opening tending to open and close depending on whether this plug is located in one or the other of the cylindrical zones mentioned.
• FIG. 12 illustrates an alternative embodiment of the bulb 10 '' comprising in this case a cylindrical zone of single narrowed circular section 2T 'of slightly conical shape. This achievement can be advantageous to facilitate the extraction of a core for forming glass and incidentally to reinforce the compression of the movable intermediate plug during the storage phase.
• the constructive characteristics of the movable intermediate plug could also be applied to the shutter member of the pis ⁇ ton-valve.
• a polygonal or elliptical or other shape with variable surface depending on whether the member is in a cylindrical zone of narrowed circular section or a cylindrical zone of wide circular section, would make it possible to reduce the dead volume of the system and decrease the diameter tolerance issues of the mixing chamber.
• this embodiment guarantees the safe operation of the piston-valve under all conditions of manufacturing tolerances.
• the ampoule advantageously comprises a closed bottom made in one piece with the body, preferably made of glass.
• the ampoule preferably has a bottom closed by a plug 40 (see fig. 11) which is fixed by means of a crimping 41 adapted on an annular bead 42 integral with the 'corresponding end of the bulb.
• a plug 40 see fig. 11
• the installation of a very fine powder in the first compartment would necessarily result in a powder deposit along the walls of the bulb, deposit which would affect the sealing of the movable intermediate plug.
• this movable intermediate stopper when the powder is already introduced into the bulb, would cause turbulence raising part of the powder deposited at the bottom and also risking damaging the tightness of said stopper. This is the reason why it is advantageous, in this case, to put in place first of all the movable intermediate plug, then the closure plug 40 which is then permanently fixed by crimping, since it does not play no more role during the operation of the system.
• the use phase comprises two successive stages: during a first stage, the liquid component passes from the second compartment into the mixing chamber which is in fact the compartment furthest from the open end of the bulb, and during a second stage the liquid mixture passes from the first compartment through the Days of the movable intermediate plug to be discharged through the single orifice of the bulb. Consequently, a double transfer is observed through the movable intermediate plug, this double transfer being authorized by the particular geometry of the intermediate plug combined with a particular geometry of the bulb.
• the system has only two active shutter elements.
• the bulb has only a single orifice during use.

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• Health & Medical Sciences (AREA)
• Engineering & Computer Science (AREA)
• Hematology (AREA)
• Anesthesiology (AREA)
• Biomedical Technology (AREA)
• Heart & Thoracic Surgery (AREA)
• Life Sciences & Earth Sciences (AREA)
• Animal Behavior & Ethology (AREA)
• General Health & Medical Sciences (AREA)
• Public Health (AREA)
• Veterinary Medicine (AREA)
• Vascular Medicine (AREA)
• Mechanical Engineering (AREA)
• Medical Preparation Storing Or Oral Administration Devices (AREA)
• Infusion, Injection, And Reservoir Apparatuses (AREA)

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• 1986
  • 1986-04-10 CH CH1413/86A patent/CH666870A5/fr not_active IP Right Cessation
• 1987
  • 1987-03-23 EP EP87902470A patent/EP0295265B1/fr not_active Expired - Lifetime
  • 1987-03-23 US US07/143,078 patent/US4941876A/en not_active Expired - Fee Related
  • 1987-03-23 JP JP62502610A patent/JPH01502086A/ja active Granted
  • 1987-03-23 WO PCT/EP1987/000163 patent/WO1987006141A1/fr active IP Right Grant
  • 1987-04-10 CA CA000534462A patent/CA1291074C/fr not_active Expired - Lifetime

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