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EP1224072A1 - Method for the production of opthalmic devices - Google Patents

Method for the production of opthalmic devices

Info

Publication number
EP1224072A1
EP1224072A1 EP00966300A EP00966300A EP1224072A1 EP 1224072 A1 EP1224072 A1 EP 1224072A1 EP 00966300 A EP00966300 A EP 00966300A EP 00966300 A EP00966300 A EP 00966300A EP 1224072 A1 EP1224072 A1 EP 1224072A1
Authority
EP
European Patent Office
Prior art keywords
spin casting
ophthalmic device
mould
methacrylate
casting mould
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.)
Withdrawn
Application number
EP00966300A
Other languages
German (de)
French (fr)
Inventor
Howard Stephen Sutton
Wade Marcel Tipton
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Clearlab UK Ltd
Original Assignee
Hydron 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 Hydron Ltd filed Critical Hydron Ltd
Publication of EP1224072A1 publication Critical patent/EP1224072A1/en
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
    • B29D11/00—Producing optical elements, e.g. lenses or prisms
    • B29D11/00951—Measuring, controlling or regulating
    • B29D11/0098—Inspecting lenses
    • B29D11/0099—Inspecting lenses while still attached to the mould
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
    • B29C41/02—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of definite length, i.e. discrete articles
    • B29C41/04—Rotational or centrifugal casting, i.e. coating the inside of a mould by rotating the mould
    • B29C41/042—Rotational or centrifugal casting, i.e. coating the inside of a mould by rotating the mould by rotating a mould around its axis of symmetry
    • B29C41/045—Rotational or centrifugal casting, i.e. coating the inside of a mould by rotating the mould by rotating a mould around its axis of symmetry the axis being placed vertically, e.g. spin casting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
    • B29D11/00—Producing optical elements, e.g. lenses or prisms
    • B29D11/00009—Production of simple or compound lenses
    • B29D11/00471—Production of simple or compound lenses made by rotational casting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
    • B29D11/00—Producing optical elements, e.g. lenses or prisms
    • B29D11/00009—Production of simple or compound lenses
    • B29D11/0048—Moulds for lenses
    • B29D11/00567—Moulds for lenses wherein the mould forms part of the final package for lenses
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
    • B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
    • B29C35/08—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation
    • B29C35/0888—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using transparant moulds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/0002—Condition, form or state of moulded material or of the material to be shaped monomers or prepolymers

Definitions

  • the alkyl and cycloalkyl groups contain up to 20 carbon atoms, e.g. (C ⁇ -C 2 o alkyl and C 1 -C 20 cycloalkyl) acrylates. and (C 1 -C 20 alkyl and C 1 -C 20 cycloalkyl) methacrylates.
  • typical monomers include any one of methyl acrylate. ethyl acrylate.

Landscapes

  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Ophthalmology & Optometry (AREA)
  • Eyeglasses (AREA)
  • Casting Or Compression Moulding Of Plastics Or The Like (AREA)

Abstract

The present invention provides a method of spin casting an opthalmic device the method comprising: i) polymerising one or more monomers in a spin casting mould to form the opthalmic device; and ii) sealing the opthalmic device in the spin casting mould to provide a package.

Description

METHOD FOR THE PRODUCTION OF OPTHALMIC DEVICES
The present invention relates to a method of spin casting an ophthalmic device. In particular the present invention relates to a method in which one or more monomers are polymerised in a spin casting mould to form the ophthalmic device, and the ophthalmic device is subsequently sealed in the spin casting mould to provide a package.
The unit costs for the production of ophthalmic devices, in particular contact lenses, have typically been low with respect to the period over which the device may be used. However, as with all products there has been a desire to reduce the unit cost. In the field of ophthalmic devices this desire has been increased by the provision of disposable contact lenses, such as monthly and daily disposable lenses.
GB-A-2237241 teaches that during the preparation and processing of an ophthalmic device such as a contact lens, a cost and quality advantage may be achieved by carrying out inspection, power measurement, extraction, and hydration in the cast mould in which a lens is formed. The disclosed method comprises polymerising a monomer in a mould cavity between a male mould surface in a first mould part and a female mould surface in a second mould part, opening the mould to expose the cast lens, and sealing the lens in a package. GB-A-2237241 teaches that the disclosed advantages may be achieved by opening the cast mould to expose the cast lens while supported on the male mould surface, and sealing the lens in a package by sealing a cover member on to said mould part. The male portion is that which presents the lens to the user convex surface uppermost. According to GB-A-2237241 such a presentation is an advantageous for the user and is necessary for many post-polymerisation treatments.
The cost and quality implications of transferring lenses after polymerisation has also been addressed in the art by the provision of release agents, see for example WO 95/1 1789 which discloses a release solution comprising isopropanol.
In a first aspect the present invention provides a method of spin casting an ophthalmic device the method comprising, (i) polymerising one or more monomers by spin casting in a spin casting mould to form the ophthalmic device, and (ii) sealing the ophthalmic device in the spin casting mould to provide a package.
The present invention is advantageous as it provides a simple method for manufacture and packaging of ophthalmic devices. The present invention provides for a one piece mould and container which carries the device throughout the manufacturing process. The present invention does not require the complex apparatus of cast moulding methods. Yet further because a one piece mould is utilised the present invention does not require the complex control which is required in cast moulding to ensure that the ophthalmic device is held on the required portion of the two piece mould.
Spin casting is a process known in the art. for example in US-A-4516924, US-A- 4517138. US-A-4517140, US-A-4551086, US-A-4534723, US-A-4584148, US-A- 5076683, US-A-5260001, and US-A-4719248. The process provides a concave mould comprising a single portion into which monomer in dosed. The mould is spun at high speed and the monomer is cured. Polymerisation is typically initiated by UV irradiation.
It will be appreciated therefore, that the spin casting process/package of the present invention is utilises a single mould portion. The lens is presented in the mould concave side upper most.
Preferably the polymerisation of the monomer of the present invention is initiated by UV irradiation.
Once the ophthalmic device has been formed the treatment(s) necessary to prepare a device suitable for wear is/are performed on the device whilst present in the mould. For example, the device may be hydrated and/or tinted. Thus in a preferred aspect the method of the present invention comprises the further step of hydrating the polymerised monomer prior to the sealing of the spin casting mould to provide a package. Preferably the hydration is performed by contacting the polymerised monomer with a hydration solution containing a surfactant.
The presence of a surfactant in the hydration solution will assist in the prevention and/or inhibition of differential hydration of the polymer. After polymerisation, the polymer will be adhered to the spin casting mould. On hydration. the polymer will separate from the mould. Differential hydration may lead to areas of the device which have different thicknesses to each other separating from the mould at different rates. This may lead to stresses in the device which damage the optical surface of the device. Such damage may lead to a hazy appearance on the surface of the device.
The one or more monomers of the present invention are selected to provide a device having the desired final properties. Suitable monomers include one of: (alkyl and cycloalkyl) acrylates; (alkyl and cycloalkyl) methacrylates; free-radical polymerisable olefinic acids. including alkoxy-, alkylphenoxy-, alkylphenoxy-(polyethyleneoxide)-, vinyl ester-, amine substituted (including quaternary ammonium salts thereof), nitrile-, halo-, hydroxy-, and acid substituted (for example phospho- or sulpho-) derivatives thereof; and other suitable ethylenically unsaturated polymerisable moieties; including combinations thereof. Preferably the alkyl and cycloalkyl groups contain up to 20 carbon atoms, e.g. (Cι-C2o alkyl and C1-C20 cycloalkyl) acrylates. and (C1-C20 alkyl and C1-C20 cycloalkyl) methacrylates. In more detail, typical monomers include any one of methyl acrylate. ethyl acrylate. n- propyl acrylate, isopropyl acrylate, n-butyl acrylate, isobutyl acrylate, t-butyl acrylate, isobornyl acrylate, pentyl acrylate, hexyl acrylate, octyl acrylate, iso-octyl acrylate, nonyl acrylate, lauryl acrylate. stearyl acrylate, eicosyl acrylate, 2-ethylhexyl acrylate, cyclohexyl acrylate, cycloheptyl acrylate, methyl methacrylate, ethyl methacrylate. hydroxymethylacrylate. hydroxymethylmethacrylate, propyl methacrylate, n-butyl methacrylate. t-butyl methacrylate. isobutyl methacrylate. pentyl methacrylate, hexyl methacrylate, cyclohexyl methacrylate, 2-ethylhexyl methacrylate, isobornyl methacrylate, heptyl methacrylate, cycloheptyl methacrylate, octyl methacrylate, iso-octyl methacrylate, nonyl methacrylate. decyl methacrylate, lauryl methacrylate, eicosyl methacrylate, dodecyl acrylate, pentadecyl acrylate, cetyl acrylate, stearyl acrylate, eicosyl acrylate, isodecyl acrylate, vinyl stearate, nonylphenoxy-(ethyleneoxide)ι.2o acrylate, octadecene, hexadecene, tetradecene, dodecene, dodecyl methacrylate, pentadecyl methacrylate, cetyl methacrylate, stearyl methacrylate. eicosyl methacrylate, isodecyl methacrylate. nonylphenoxy- (ethyleneoxide)ι-20 methacrylate, acrylic acid, methacrylic acid, fumaric acid, crotonic acid, itaconic acid, fumaric anhydride, crotonic anhydride, itaconic anhydride, maleic acid, maleic anhydride, styrene, alpha-methyl styrene, vinyl toluene, acrylonitrile, methacrylonitrile, ethylene, vinyl acetate, vinyl chloride, vinylidene chloride, acrylamide. methacrylamide. methacrylamide 2-cyanoethyl acrylate, 2-cyanoethyl methacrylate. dimethylaminoethyl methacrylate, dimethylaminopropyl methacrylate t-butylaminoethyl methacrylate. glycidyl acrylate, glycidyl methacrylate. glyceryl acrylate. glyceryl methacrylate. benzyl acrylate. benzyl methacrylate. phenyl acrylate, phenyl methacrylate. vinyl pyridine, vinyl pyrrolidine, siloxanes, silanes and mixtures thereof. Other polymerisable monomers are disclosed in US-A-2879178. US-A-3037006. US-A-3502627, US-A-3037969 and US-A-3497485.
Preferred monomers include any one of glyceryl methacrylate (GMA), (2,2 dimethyl- 1.3-dioxolan-4-yl) methyl methacrylate (GMAK), hydroxy ethyl methacrylate (HEMA), methacrylic acid, acrylic acid, GYMA. N-vinyl pyrrolidone, alkyl methacrylates (such as C i-20 alkyl methacrylates. more preferably C M S alkyl methacrylates, more preferably C MO alkyl methacrylates. more preferably Ci-s alkyl methacrylates, such as methyl methacrylate), alkyl acrylates (such as C ι-2o alkyl acrylates, more preferably C M alkyl acrylates. more preferably C 0 alkyl acrylates, more preferably C |-5 alkyl acrylates. such as methyl acrylate), aryl methacrylates, aryl acrylates, diacetone acrylamide, acrylamide. methacrylamide. N-alkyl acrylamides (such as Ci-20 N-alkyl acrylamides. more preferably C ι-t5 N-alkyl acry lamides. more preferably C MO N-alkyl acrylamides. more preferably C1-5 N-alkyl acrylamides. such as methyl acrylamide), N-alkyl methacrylamides (such as Ci-20 N-alkyl methacrylamides, more preferably C M . N-alkyl methacrylamides. more preferably C O N-alkyl methacrylamides. more preferably C\.$ N-alkyl methacrylamides. such as methyl methacrylamide), vinyl acetate, vinyl esters, styrene, other substituted olefms. N- dialkyl acrylamides (such as Ci-20 N-dialkyl acrylamides. more preferably C M N-dialkyl acrylamides. more preferably C MO N-dialkyl acrylamides, more preferably C|-s N-dialkyl acrylamides. such as N N dimethyl acrylamide), N-dialkyl methacrylamides (such as C1.20 N-dialkyl methacrylamides. more preferably C M5 N-dialkyl methacrylamides, more preferably C M 0 N-dialkyl methacrylamides, more preferably .s N-dialkyl methacrylamides. such as N N dimethyl methacrylamide), 3-methacryloxypropyl tris (trimethysilyl siloxy) silane (TRIS monomer), fluoro substituted alkyl and aryl acrylates and methacrylates (preferably wherein the alkyl is Cι-20 alkyl, more preferably C M 5 alkyl, more preferably C MO alkyl. more preferably C1.5 alkyl), and combinations thereof. More preferred monomers include any one of glyceryl methacrylate (GMA), (2,2 dimethyl- l,3-dioxolan-4-yl) methyl methacrylate (GMAK). 2-hydroxy ethyl methacrylate (2- HEMA), methacrylic acid, acrylic acid and glycidyl methacrylate. or combinations thereof.
The lists of monomers also include substituted derivatives of those monomers, such as halogenated monomers, especially fluorinated monomer derivatives, and acetal and ketal derivatives.
In a preferred aspect the one or more monomers are selected from glyceryl methacrylate (GMA), 2-hydroxy ethyl methacrylate (2-HEMA). and mixtures thereof. Preferably the one or more monomers are selected from a mixture of 2-HEMA and GMA. Preferably the one or more monomers consist essentially of 2-HEMA and or GMA. Preferably the one or more monomers consist essentially of a mixture of 2-HEMA and GMA. In this aspect the monomers may be the monomers disclosed in US-A-4038264.
In a further preferred aspect the mould are configured such that they are stackable. In this aspect the present invention is further advantageous. Use of a single mould portion during formation of the device allows one to design the mould to be stackable with similar moulds. When a two part mould system is used, as is required by cast moulding, the mould configuration is determined by its relationship would the other mould portion. Thus the present invention may further provided a plurality of packages which are stacked together. Preferably, the stackable packages are as described in WO 99/11529.
The present invention provides a packaged ophthalmic device prepared in accordance with a method described herein.
Yet further the present invention provides an article comprising a spin casting mould containing an ophthalmic device, wherein the ophthalmic device is ready for wear and is sealed in the spin casting mould
As described above, the articles may be stacked. Thus the present invention further provides a plurality of articles as described herein wherein the articles are in a stacked configuration. The material from which the spin casting mould and hence final packaging is formed may be selected depending on the properties required during production, storage and/or use. In the process of the present invention the material is preferably selected such that the spin casting mould is transparent or translucent. A transparent or translucent mould allows for inspection of lens whilst located in mould and thereby allows automatic inspection of the lens. Moreover inspection of the lens without the need to remove the same from the mould packaging avoids the risks of contamination and/or damage.
Thus in a further preferred aspect the method of the present invention comrpises the further step of inspecting the opthalmic device whilst in the spin casting mould.
Suitable materials for the formation of the spin casting mould include polyvinyl chloride, polypropylene, derivatives and mixtures thereof.
The spin casting process of the present invention is yet further advantageous as it allows for the preparation of a toric ophthalmic device having the advantages described above. Spin casting is particularly employed for the preparation of toric devices. Thus the prior art processes using for example cast moulding have not been able to provide a satisfactory toric device. Preferably the ophthalmic device of the present invention has a toric configuration.
EXAMPLE
A contact lens was prepared by spin casting in accordance with the following procedure
Spin casting moulds were provided formed from polypropylene. The moulds were translucent.
The amount of initiated monomer (a mixture of 2-HEMA and GMA in a ratio of 1 : 1) required in the casts for the power of lens required was identified from tabulated fabrication data. The monomer was dispensed into the casts using a Hamilton volumetric syringe. The filled cats were transferred to a wetting apparatus for no more than 30 minutes A spin casting machine available from Concept Design and Engineering, Gosport (UK) was started up in accordance with standard procedure. The required spin speed was ascertained in the fabrication data for the power of lens required an was set and checked with a tachometer. The cycle time was set for 30 seconds ± 2 seconds.
Filled casts were removed from the wetting apparatus and were placed in the loading mechanism. The spinning motor was switched on and the cycle started.
The lenses were cured during spinning by UV irradiation.
The spun and cured lenses were hydrated with a packaging solution consisting of a phosphate buffered saline solution. The lenses were allowed to stand in the solution until they had hydrated and released from the mould. The solution was removed and a further portion of the solution was added to the mould.
The moulds were then forwarded to a packaging line. On the packaging line a foil/polymer laminate film was adhered to the outer rim of each mould. The film was trimmed and the lenses forwarded for inspection. The translucency of the mould allowed for inspection through the '"bottom portion" of the mould.
All publications mentioned in the above specification are herein incorporated by reference. Various modifications and variations of the described methods and system of the invention will be apparent to those skilled in the art without departing from the scope and spirit of the invention. Although the invention has been described in connection with specific preferred embodiments, it should be understood that the invention as claimed should not be unduly limited to such specific embodiments. Indeed, various modifications of the described modes for carrying out the invention which are obvious to those skilled in chemistry or related fields are intended to be within the scope of the following claims.

Claims

1. A method of spin casting an ophthalmic device the method comprising,
(i) polymerising one or more monomers in a spin casting mould to form the ophthalmic device, and
(ii) sealing the ophthalmic device in the spin casting mould to provide a package.
2. A method according to claim 1 wherein the method comprises the further step of inspecting the ophthalmic device whilst in the spin casting mould.
3. A method according to claim 1 or 2 wherein the polymerised monomer is hydrated prior to the sealing of the spin casting mould to provide a package.
4. A method according to claim 3 wherein the hydration is performed by contacting the polymerised monomer with a hydration solution containing a surfactant.
5. A method according to any one of claims 1 to 4 wherein the polymerisation of the monomer is initiated by UV irradiation.
6. A method according to any one of claims 1 to 5 wherein the one or more monomers are selected from HEMA, GMA and mixtures thereof.
7. A method according to any one of claims 1 to 6 wherein a plurality of packages are provided and subsequently stacked together.
8. A packaged ophthalmic device prepared in accordance with the method of any one of claims 1 to 7.
9. An article comprising a spin casting mould containing an ophthalmic device, wherein the ophthalmic device is ready for wear and is sealed in the spin casting mould
10. A plurality of articles as defined in claim 9 wherein the articles are in stacked configuration.
1 1. The invention of any one of claims 1 to 10 wherein the spin casting mould is transparent or translucent.
12. The invention of any one of claims 1 to 1 1 wherein the spin casting mould is formed from a material selected from polyvinyl chloride, polypropylene, derivatives and mixtures thereof.
13. The invention of any one of claims 1 to 12 wherein the ophthalmic device has a toric configuration.
14. A method of spin casting an ophthalmic device as substantially described herein with reference to the Example.
15. A packaged ophthalmic device as substantially described herein with reference to the Example.
16. An article comprising a spin casting mould containing an ophthalmic device as substantially described herein with reference to the Example.
EP00966300A 1999-10-25 2000-10-09 Method for the production of opthalmic devices Withdrawn EP1224072A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
GB9925202A GB2355686A (en) 1999-10-25 1999-10-25 A method of forming an ophthalmic device
GB9925202 1999-10-25
PCT/GB2000/003875 WO2001030559A1 (en) 1999-10-25 2000-10-09 Method for the production of opthalmic devices

Publications (1)

Publication Number Publication Date
EP1224072A1 true EP1224072A1 (en) 2002-07-24

Family

ID=10863323

Family Applications (1)

Application Number Title Priority Date Filing Date
EP00966300A Withdrawn EP1224072A1 (en) 1999-10-25 2000-10-09 Method for the production of opthalmic devices

Country Status (4)

Country Link
EP (1) EP1224072A1 (en)
AU (1) AU7674400A (en)
GB (1) GB2355686A (en)
WO (1) WO2001030559A1 (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CZ298423B6 (en) * 2004-11-24 2007-09-26 Wilens, Spol. S R. O. Process for producing intraocular lenses by polymerization mold casting

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1143518A (en) * 1979-01-15 1983-03-29 George T. Croft Method and apparatus for making plastic lenses
GB2237241B (en) * 1988-11-02 1993-01-13 Nat Res Dev Contact lens cast moulding and packaging
US5066431A (en) * 1990-04-20 1991-11-19 Briggs Charles R Method of making toric contact lenses
SG49612A1 (en) * 1993-07-19 2003-03-18 Novartis Ag A process and device for the manufacture of moulding and mouldings manufactured in accordance with that process
TW325744U (en) * 1993-07-21 1998-01-21 Ciba Geigy Ag Two-sided contact lens mold
WO1995011789A1 (en) * 1993-10-28 1995-05-04 Bausch & Lomb Incorporated Method of releasing contact lenses from the mold
TW295570B (en) * 1994-05-04 1997-01-11 Ciba Geigy Ag
GB2328924A (en) * 1997-09-04 1999-03-10 Hydron Ltd Stackable containers

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO0130559A1 *

Also Published As

Publication number Publication date
GB9925202D0 (en) 1999-12-22
AU7674400A (en) 2001-05-08
GB2355686A (en) 2001-05-02
WO2001030559A1 (en) 2001-05-03

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