WO1998002240A1 - Preservation by foam formation - Google Patents
Preservation by foam formation Download PDFInfo
- Publication number
- WO1998002240A1 WO1998002240A1 PCT/US1997/012156 US9712156W WO9802240A1 WO 1998002240 A1 WO1998002240 A1 WO 1998002240A1 US 9712156 W US9712156 W US 9712156W WO 9802240 A1 WO9802240 A1 WO 9802240A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- foam
- drying
- biologically active
- vacuum
- temperature
- 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.)
- Ceased
Links
Classifications
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- C12N9/00—Enzymes; Proenzymes; Compositions thereof; Processes for preparing, activating, inhibiting, separating or purifying enzymes
- C12N9/0004—Oxidoreductases (1.)
- C12N9/0006—Oxidoreductases (1.) acting on CH-OH groups as donors (1.1)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- C12N1/00—Microorganisms; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor
- C12N1/04—Preserving or maintaining viable microorganisms
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- C12N9/00—Enzymes; Proenzymes; Compositions thereof; Processes for preparing, activating, inhibiting, separating or purifying enzymes
- C12N9/96—Stabilising an enzyme by forming an adduct or a composition; Forming enzyme conjugates
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S516/00—Colloid systems and wetting agents; subcombinations thereof; processes of
- Y10S516/924—Significant dispersive or manipulative operation or step in making or stabilizing colloid system
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2984—Microcapsule with fluid core [includes liposome]
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/10—Composition for standardization, calibration, simulation, stabilization, preparation or preservation; processes of use in preparation for chemical testing
- Y10T436/107497—Preparation composition [e.g., lysing or precipitation, etc.]
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/10—Composition for standardization, calibration, simulation, stabilization, preparation or preservation; processes of use in preparation for chemical testing
- Y10T436/108331—Preservative, buffer, anticoagulant or diluent
Definitions
- the invention relates to methods for preserving sensitive biologically active solutes and suspensions, emulsions and dispersions of, for example, enzymes, proteins, viruses, serums, vaccines, liposomes and cell suspensions .
- the present invention is a method of preserving sensitive biological suspensions and solutions by forming stable foams from fluid materials to be dried, as an aid both to the drying of one or more biologically active substrates in the fluid and as an aid in preparing an easily soluble dried product suitable for further commercial use.
- the stable foams are formed by partially removing water in the biologically active sample to form a viscous liquid and by further subjecting the reduced liquid to vacuum to cause it to "boil" during further drying at temperatures substantially lower than 100 degrees C.
- the present invention is a method of preserving sensitive biological dispersions, suspensions, emulsions and solutions by forming stable foams from fluid materials to be dried, as an aid both to the drying of one or more biologically active substrates in the fluid and as an aid in preparing an easily divisible dried product suitable for further commercial use.
- the stable foams are formed by partially removing the water to form a viscous liquid and by further subjecting the reduced liquid to vacuum, to cause it to "boil" during further drying at temperatures substantially lower than 100 degrees C.
- reduced pressure is applied to viscous solutions or suspensions of biologically active materials to cause the solutions or suspensions to foam during boiling, and during the foaming process further solvent removal causes the ultimate production of a stable open-cell or closed-cell foam.
- foams are easily divisible by cutting, milling or other dividing techniques, and the foaming action itself enhances water removal by maximizing liquid surface area available for evaporation.
- the solvent fraction of the materials to be dried will be aqueous, however, it should be understood that the present method may be applied to solutions and suspensions of various types including those containing nonaqueous solvents or mixture of such solvents .
- the inventive apparatus is a novel combination of a vacuum pump with a temperature controlled desiccator device.
- Optional features of such a combination include sensors for temperature measurement and heat flow control, microprocessors for calculating other process parameters based on data collected from these and other sensors and etc.
- Such a device allows implementation of a novel two- dimensional vacuum and temperature protocol for drying.
- the foam forming process includes two steps: (a) an intensive dehydration of the solution or dispersion containing the biologically active agent by boiling under vacuum, to form a stable, non-collapsing foam and (b) subsequent secondary drying of the foams, to the extent that the foams are stable and do not collapse during storage.
- the invention provides a scalable method for preserving sensitive biologically active materials (proteins, enzymes, serums, vaccines, viruses, liposomes and cell suspensions) with a uniquely engineered drying method. Using this method, it is possible to rehydrate the samples with water or aqueous solutions to reverse the process to the initial biological activity. The method may be applied for the preservation of pharmaceutical, fluid or virtually any other biologically active products or solutes.
- foams are a kinetic process and depends on the rate of temperature and vacuum changes during formation of the foam as well as the initial concentration and composition of the solution or dispersion containing the biologically active substance. Stability of the foams may be further enhanced by the addition of surfactants or other synthetic or biological polymers as long as those additives do not interfere with the biological activity of the solute intended for conversion to dry form. Secondary drying and optional cooling of the formed and initially dry foams may be conducted to assure stability of the foam during storage. Cooling may be used to convert the foamed material to the glass state. Foams prepared according to the present invention may be stored whole or subdivided or milled, and when they are to be used need only be rehydrated in order to restore their original biologic activity.
- Aqueous 50% glycerol isocitrate dehydrogenase solution from Sigma Chemical Co. containing 59.4 units of activity per ml. was dialyzed for 5 hours in 0.1 M TRIS HC1 buffer (pH 7.4).
- the activity decrease was associated with decrease in the enzyme concentration because of dilution during the dialysis.
- the samples were rehydrated with 500 microliters water. Rehydration of the samples containing dry foams was an easy process that was completed within several seconds. Reconstituted sample was assayed for activity by assaying ability to reduce NADP, measured spectrophotometrically at 340 nm.
- the activity was 2.6 +/- 0.2 units/ml. which means there was no loss of activity during drying and subsequent storage at room temperature .
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Zoology (AREA)
- Wood Science & Technology (AREA)
- Genetics & Genomics (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Biotechnology (AREA)
- Biochemistry (AREA)
- Biomedical Technology (AREA)
- Microbiology (AREA)
- Medicinal Chemistry (AREA)
- General Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Tropical Medicine & Parasitology (AREA)
- Virology (AREA)
- Micro-Organisms Or Cultivation Processes Thereof (AREA)
- Investigating Or Analysing Biological Materials (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
- Medicines That Contain Protein Lipid Enzymes And Other Medicines (AREA)
- Medicinal Preparation (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Drying Of Solid Materials (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Colloid Chemistry (AREA)
Priority Applications (10)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE0914202T DE914202T1 (de) | 1996-07-15 | 1997-07-14 | Konservierung durch schaumformung |
| EA199900268A EA001138B1 (ru) | 1996-07-15 | 1997-07-14 | Защита пенообразованием |
| JP10506201A JP2000515856A (ja) | 1996-07-15 | 1997-07-14 | 泡沫形成による保存 |
| AU36606/97A AU714328B2 (en) | 1996-07-15 | 1997-07-14 | Preservation by foam formation |
| IL12797197A IL127971A (en) | 1996-07-15 | 1997-07-14 | Preservation by creating foam |
| NZ333738A NZ333738A (en) | 1996-07-15 | 1997-07-14 | Shelf preservation of biological active material by forming a mechanically stable foam thereof |
| BR9711808-7A BR9711808A (pt) | 1996-07-15 | 1997-07-14 | Preservação através de formação de espuma. |
| HU9903917A HUP9903917A3 (en) | 1996-07-15 | 1997-07-14 | Preservation by foam formation |
| EP97933415A EP0914202A4 (en) | 1996-07-15 | 1997-07-14 | CONSERVATION THROUGH FOAM FORMING |
| NO990158A NO990158D0 (no) | 1996-07-15 | 1999-01-14 | Konservering ved skumdannelse |
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US2179696P | 1996-07-15 | 1996-07-15 | |
| US60/021,796 | 1996-07-15 | ||
| US08/785,473 US5766520A (en) | 1996-07-15 | 1997-01-17 | Preservation by foam formation |
| US08/785,473 | 1997-01-17 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| WO1998002240A1 true WO1998002240A1 (en) | 1998-01-22 |
| WO1998002240B1 WO1998002240B1 (en) | 1998-03-05 |
Family
ID=26695104
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/US1997/012156 Ceased WO1998002240A1 (en) | 1996-07-15 | 1997-07-14 | Preservation by foam formation |
Country Status (18)
| Country | Link |
|---|---|
| US (1) | US5766520A (enExample) |
| EP (1) | EP0914202A4 (enExample) |
| JP (1) | JP2000515856A (enExample) |
| KR (1) | KR100457748B1 (enExample) |
| CN (1) | CN1116104C (enExample) |
| AU (1) | AU714328B2 (enExample) |
| BR (1) | BR9711808A (enExample) |
| CA (1) | CA2260233A1 (enExample) |
| CZ (1) | CZ7999A3 (enExample) |
| DE (1) | DE914202T1 (enExample) |
| EA (1) | EA001138B1 (enExample) |
| HU (1) | HUP9903917A3 (enExample) |
| IL (1) | IL127971A (enExample) |
| NO (1) | NO990158D0 (enExample) |
| NZ (1) | NZ333738A (enExample) |
| PL (1) | PL331174A1 (enExample) |
| TR (1) | TR199900127T2 (enExample) |
| WO (1) | WO1998002240A1 (enExample) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999027071A1 (en) * | 1997-11-26 | 1999-06-03 | Universal Preservation Technologies, Inc. | Preservation of sensitive biological samples by vitrification |
| WO2000040696A1 (en) * | 1999-01-05 | 2000-07-13 | Universal Preservation Technologies, Inc. | Preservation of sensitive biological materials at ambient temperatures by vitrification |
| WO2000066710A3 (en) * | 1999-05-04 | 2001-02-08 | Eric Edward Worrall | Method for the preservation of viruses and mycoplasma |
| WO2001037804A3 (en) * | 1999-11-22 | 2001-11-22 | Universal Preservation Technologies Inc | Preservation and formulation of bioactive materials |
| WO2002000201A3 (en) * | 2000-06-27 | 2002-04-18 | Hoffmann La Roche | Method for preparing a composition |
| US6537666B1 (en) | 2000-10-23 | 2003-03-25 | Universal Preservation Technologies, Inc. | Methods of forming a humidity barrier for the ambient temperature preservation of sensitive biologicals |
| US6692695B1 (en) | 1999-05-06 | 2004-02-17 | Quadrant Drug Delivery Limited | Industrial scale barrier technology for preservation of sensitive biological materials |
| US7153472B1 (en) | 2000-11-22 | 2006-12-26 | Quadrant Drug Delivery Limited | Preservation and formulation of bioactive materials for storage and delivery in hydrophobic carriers |
| EP1494651A4 (en) * | 2002-04-11 | 2010-10-13 | Medimmune Vaccines Inc | PRESERVATION OF BIOACTIVE MATERIALS WITH FREEZZED FOAM |
| US20230357807A1 (en) * | 2020-07-27 | 2023-11-09 | Karlsruher Institut Fuer Technologie | Catalytically active protein foams, and method for producing same |
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| DE69535897D1 (de) | 1994-03-07 | 2009-01-22 | Nektar Therapeutics | Verfahren und Zusammensetzung für die pulmonale Darreichung von Insulin |
| US20030113273A1 (en) * | 1996-06-17 | 2003-06-19 | Patton John S. | Methods and compositions for pulmonary delivery of insulin |
| US6290991B1 (en) | 1994-12-02 | 2001-09-18 | Quandrant Holdings Cambridge Limited | Solid dose delivery vehicle and methods of making same |
| CZ88697A3 (en) | 1994-09-22 | 1997-09-17 | Quadrant Holdings Cambridge | Composition used for re-hydration and nourishment in the course of athletic outputs and processes for preparing thereof |
| US6964771B1 (en) * | 1995-06-07 | 2005-11-15 | Elan Drug Delivery Limited | Method for stably incorporating substances within dry, foamed glass matrices |
| US6509146B1 (en) | 1996-05-29 | 2003-01-21 | Universal Preservation Technologies, Inc. | Scalable long-term shelf preservation of sensitive biological solutions and suspensions |
| US6468782B1 (en) * | 1996-12-05 | 2002-10-22 | Quadrant Healthcare (Uk) Limited | Methods of preserving prokaryotic cells and compositions obtained thereby |
| GB9705588D0 (en) | 1997-03-18 | 1997-05-07 | Anglia Research Foundation | Stable particle in liquid formulations |
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- 1997-07-14 JP JP10506201A patent/JP2000515856A/ja not_active Ceased
- 1997-07-14 CZ CZ9979A patent/CZ7999A3/cs unknown
- 1997-07-14 CA CA002260233A patent/CA2260233A1/en not_active Abandoned
- 1997-07-14 WO PCT/US1997/012156 patent/WO1998002240A1/en not_active Ceased
- 1997-07-14 KR KR10-1999-7000253A patent/KR100457748B1/ko not_active Expired - Fee Related
- 1997-07-14 HU HU9903917A patent/HUP9903917A3/hu not_active Application Discontinuation
- 1997-07-14 EA EA199900268A patent/EA001138B1/ru not_active IP Right Cessation
- 1997-07-14 NZ NZ333738A patent/NZ333738A/xx unknown
- 1997-07-14 EP EP97933415A patent/EP0914202A4/en not_active Withdrawn
- 1997-07-14 TR TR1999/00127T patent/TR199900127T2/xx unknown
- 1997-07-14 AU AU36606/97A patent/AU714328B2/en not_active Ceased
- 1997-07-14 CN CN97196422A patent/CN1116104C/zh not_active Expired - Fee Related
- 1997-07-14 DE DE0914202T patent/DE914202T1/de active Pending
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| WO1999027071A1 (en) * | 1997-11-26 | 1999-06-03 | Universal Preservation Technologies, Inc. | Preservation of sensitive biological samples by vitrification |
| US6306345B1 (en) | 1998-05-06 | 2001-10-23 | Universal Preservation Technologies, Inc. | Industrial scale barrier technology for preservation of sensitive biological materials at ambient temperatures |
| WO2000040696A1 (en) * | 1999-01-05 | 2000-07-13 | Universal Preservation Technologies, Inc. | Preservation of sensitive biological materials at ambient temperatures by vitrification |
| WO2000066710A3 (en) * | 1999-05-04 | 2001-02-08 | Eric Edward Worrall | Method for the preservation of viruses and mycoplasma |
| US6692695B1 (en) | 1999-05-06 | 2004-02-17 | Quadrant Drug Delivery Limited | Industrial scale barrier technology for preservation of sensitive biological materials |
| WO2001037804A3 (en) * | 1999-11-22 | 2001-11-22 | Universal Preservation Technologies Inc | Preservation and formulation of bioactive materials |
| US6534087B2 (en) | 2000-06-27 | 2003-03-18 | Hoffmann-La Roche Inc. | Process for preparing a pharmaceutical composition |
| WO2002000201A3 (en) * | 2000-06-27 | 2002-04-18 | Hoffmann La Roche | Method for preparing a composition |
| US7074431B2 (en) * | 2000-06-27 | 2006-07-11 | Hoffmann-La Roche Inc. | Process for preparing a pharmaceutical composition |
| HRP20021009B1 (hr) * | 2000-06-27 | 2011-07-31 | F. Hoffmann - La Roche Ag | Postupak za pripremu pripravka |
| US6537666B1 (en) | 2000-10-23 | 2003-03-25 | Universal Preservation Technologies, Inc. | Methods of forming a humidity barrier for the ambient temperature preservation of sensitive biologicals |
| US7153472B1 (en) | 2000-11-22 | 2006-12-26 | Quadrant Drug Delivery Limited | Preservation and formulation of bioactive materials for storage and delivery in hydrophobic carriers |
| EP1494651A4 (en) * | 2002-04-11 | 2010-10-13 | Medimmune Vaccines Inc | PRESERVATION OF BIOACTIVE MATERIALS WITH FREEZZED FOAM |
| US8067017B2 (en) | 2002-04-11 | 2011-11-29 | Medimmune, Llc | Preservation of bioactive materials by freeze dried foam |
| US8343518B2 (en) | 2002-04-11 | 2013-01-01 | Medimmune, Llc | Preservation of bioactive materials by freeze dried foam |
| EP2591771A1 (en) * | 2002-04-11 | 2013-05-15 | MedImmune, LLC | Preservation of bioactive materials by freeze dried foam |
| US20230357807A1 (en) * | 2020-07-27 | 2023-11-09 | Karlsruher Institut Fuer Technologie | Catalytically active protein foams, and method for producing same |
Also Published As
| Publication number | Publication date |
|---|---|
| NZ333738A (en) | 2000-09-29 |
| US5766520A (en) | 1998-06-16 |
| HUP9903917A2 (hu) | 2000-03-28 |
| KR20000023779A (ko) | 2000-04-25 |
| AU3660697A (en) | 1998-02-09 |
| CN1226842A (zh) | 1999-08-25 |
| EP0914202A4 (en) | 2004-09-01 |
| BR9711808A (pt) | 2000-01-18 |
| NO990158L (no) | 1999-01-14 |
| JP2000515856A (ja) | 2000-11-28 |
| CZ7999A3 (cs) | 1999-11-17 |
| IL127971A (en) | 2001-09-13 |
| EA199900268A1 (ru) | 1999-10-28 |
| IL127971A0 (en) | 1999-11-30 |
| PL331174A1 (en) | 1999-06-21 |
| TR199900127T2 (xx) | 1999-04-21 |
| AU714328B2 (en) | 1999-12-23 |
| EA001138B1 (ru) | 2000-10-30 |
| EP0914202A1 (en) | 1999-05-12 |
| NO990158D0 (no) | 1999-01-14 |
| CN1116104C (zh) | 2003-07-30 |
| HUP9903917A3 (en) | 2000-06-28 |
| KR100457748B1 (ko) | 2004-11-17 |
| CA2260233A1 (en) | 1998-01-22 |
| DE914202T1 (de) | 2000-02-17 |
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