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AU2003269064C1 - Method for producing an avocado leaf extract rich in furanic lipids - Google Patents

Method for producing an avocado leaf extract rich in furanic lipids Download PDF

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AU2003269064C1
AU2003269064C1 AU2003269064A AU2003269064A AU2003269064C1 AU 2003269064 C1 AU2003269064 C1 AU 2003269064C1 AU 2003269064 A AU2003269064 A AU 2003269064A AU 2003269064 A AU2003269064 A AU 2003269064A AU 2003269064 C1 AU2003269064 C1 AU 2003269064C1
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plant extract
producing
leaves
avocado
furanic lipids
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AU2003269064A
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AU2003269064A1 (en
AU2003269064B2 (en
Inventor
Jacques Legrand
Antoine Piccirilli
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Laboratoires Expanscience SA
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Laboratoires Expanscience SA
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Priority claimed from FR0209666A external-priority patent/FR2843027B1/en
Priority claimed from US10/206,995 external-priority patent/US6733795B2/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D307/00Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/02Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
    • C07D307/34Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS OR COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings or cooking oils
    • A23D9/007Other edible oils or fats, e.g. shortenings or cooking oils characterised by ingredients other than fatty acid triglycerides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/54Lauraceae (Laurel family), e.g. cinnamon or sassafras
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/02Stomatological preparations, e.g. drugs for caries, aphtae, periodontitis
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P17/00Drugs for dermatological disorders
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P19/00Drugs for skeletal disorders
    • A61P19/02Drugs for skeletal disorders for joint disorders, e.g. arthritis, arthrosis
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/04Pretreatment of vegetable raw material
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Veterinary Medicine (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Medicinal Chemistry (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Medical Informatics (AREA)
  • Epidemiology (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mycology (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Microbiology (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Physical Education & Sports Medicine (AREA)
  • Immunology (AREA)
  • Orthopedic Medicine & Surgery (AREA)
  • Rheumatology (AREA)
  • Dermatology (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Fats And Perfumes (AREA)
  • Furan Compounds (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Compounds Of Unknown Constitution (AREA)

Description

r 4i IN THE MATTER OF AN AUSTRALIAN Application corresponding to PCT Application PCT/FR2003/ 002377 I, Francis AHNER, c/o CABINET REGIMBEAU, of 20 rue de Chazelles, F-75847 PARIS CEDEX 17, FRANCE, do solemnly and sincerely declare that I am conversant with the English and French languages and that to the best of my knowledge and belief the following is a true and correct translation of the PCT Application filed under No. PCT/ FR2003/ 002377.
Date February 10, 2004 Francis AHNER 004920303 1 0 METHOD FOR PRODUCING AN AVOCADO LEAF EXTRACT c RICH IN FURANIC LIPIDS ct The present invention relates to a method for producing an avocado leaf plant extract rich in furanic lipids.
5 Avocado comprises, in a known manner, particular lipids of the furan type, 0 whose main component is a linoleic furan: Thus, the expression "avocado furanic lipids" is understood to mean according to the invention the components corresponding to the formula:
IR
0 in which R is a linear C 11
-C
19 preferably C 13
-C
17 hydrocarbon chain which is saturated or which comprises one or more ethylenic or acetylenic unsaturations. These avocado furanic lipids have been described in particular in Farines, M et al, 1995, J. of Am. Oil Chem. Soc. 72, 473.
Currently, the known routes of synthesis for producing furanic lipids and the routes commonly used starting from avocados in the form of fruits as raw material.
Given the therapeutic value of avocado furanic lipids for their beneficial and curative action on the connective tissue, in particular in inflammatory pathologies such as osteoarthritis, periodontitis and scleroderma, and their high cost in general, a strong interest therefore exists in finding alternative routes for preparing these avocado furanic lipids.
The Applicant has thus developed a method which makes it possible to obtain an avocado leaf plant extract rich in furanic lipids, namely having a content ranging from to 80%, and preferably 30 to 004920303 2 O This method, in which the raw material consists of avocado leaves, comprises cI the following steps: a liquid-solid extraction step followed by evaporation under vacuum, and a heat treatment step between 80 and 120 0
C.
5 These two steps may be carried out in this order or in the reverse order.
NO The avocado leaves may be obtained from avocado plants belonging to the following varieties: Hass, Fuerte, Ettinger, Bacon, Nabal, Anaheim, Lula, Reed, Zutano, Queen, Criola Selva, Mexicana Canta, Region Dschang, Hall, Booth, Peterson, Collinson Red or Alpha Krome and more particularly to the varieties Hass, Fuerte and 0 Reed.
Several solvents may be used during the step of liquid-solid extraction of the leaves, having previously been optionally subjected to dehydration. The solvents may be chosen from the group consisting of alkanes, halogenated alkanes, ethers, esters, alcohols, aromatic compounds and supercritical fluids. Hexane, ethanol, methanol, chloroform, dichloromethane and ethyl acetate are preferred, alone or in the form of a mixture.
The heat treatment step, whether it takes place directly on the leaves or at the plant extract stage, is carried out at temperatures of between 80 and 120 0 C. This heat treatment may last from 5 to 72 hours.
According to the method of the invention, the heat treatment step may be performed in the presence or otherwise of an acid catalyst.
The expression acid catalysts is understood to mean in a broad sense socalled homogeneous inorganic or organic catalysts such as hydrochloric, sulphuric, acetic or para-toluenesulphonic acids, but also, and preferably, heterogeneous solid catalysts such as silica, alumina, silicas-aluminas, zirconias, zeolites and acidic resins.
Acidic aluminas with large specific surface areas, that is to say at least equal to 200 m2/g, will be chosen in particular.
004920303 3 The method may also comprise a step, prior to the liquid-solid extraction, of dehydration of avocado leaves.
The expression dehydration of the avocado leaves is understood to mean more generally all the techniques known to persons skilled in the art which make it possible to extract water from a compound. Among these techniques, there may be mentioned drying under a hot air stream or under a controlled atmosphere (e.g.
nitrogen) at atmospheric pressure or under vacuum, in a thick layer or in a thin layer, but also microwave drying, spray-drying, freeze-drying and osmotic dehydration in solution (direct osmosis) or in solid phase drying in osmotic bags).
0 In general, the temperature during this dehydration step will be preferably maintained, whatever the technique used, at less than or equal to 80 0
C.
Moreover, it is preferable, in the context of the present invention, to stop the dehydration when the residual moisture reaches the level of In the context of the present invention, for the sake of ease of industrial implementation and for cost considerations, drying in ventilated dryers, in a thin layer and under a hot air stream, at a temperature of between 70 and 750C. is preferred. The duration of the operation may vary from 5 to 72 hours.
According to a first variant, the method is carried out according to the succession of steps below: Step 1: heat treatment of the avocado leaves, Step 2: liquid-solid extraction of the avocado leaves, Step 3: vacuum evaporation of the solvent until a solvent-free plant extract is obtained.
According to a second variant, the method is carried out according to the succession of steps below: Step 1: liquid-solid extraction of the avocado leaves, 004920303 4 O Step 2: vacuum evaporation of the solvent until a solvent-free plant extract is N' obtained, Step 3: heat treatment of the plant extract.
According to final variant, the method is carried out according to the 5 succession of steps below: Step 1: dehydration of the avocado leaves,
NO
C Step 2: liquid-solid extraction of the avocado leaves, Step 3: vacuum evaporation of the solvent until a plant extract is obtained, Step 4: heat treatment of the plant extract.
The leaves are advantageously ground before any operation performed in the context of the method according to the invention.
The present invention finally relates to an avocado leaf plant extract which can be obtained by the method according to the invention, including according to all its variants.
The following non-limiting examples illustrate the invention.
EXAMPLE 1 One kilogram of leaves of avocado plant of the Hass variety is carefully ground. The ground product obtained (320 g) is brought into contact with 2 liters of ethanol and then heated under reflux for 5 hours. Once cool, the mixture is filtered on a Buchner funnel and the cake is washed with three times 100 ml of ethanol. The solvent is then evaporated under vacuum using a rotary evaporator, and then drawn off under vacuum for a further one hour after complete removal of the solvent. The extract obtained is then placed in an oven at 100 0 C for 24 hours, and then analysed. 23 g of extract are obtained according to this method.
The physicochemical and chromatographic analyses of this extract gave the following results: 004920303 incineration residue: <0.1% Scontent of volatile compounds: <0.1% content of furanic lipids: 42% EXAMPLE 2 .O 5 One kilogram of leaves of avocado plant of the Fuerte variety is carefully ground. The ground product obtained (305 g) is brought into contact with 2 liters of N hexane and then heated under reflux for 5 hours. Once cool, the mixture is filtered on a Buchner funnel and the cake is washed with three times 100 ml of hexane. Once assembled, the hexane-containing phases are dried in the presence of Na 2
SO
4 The 0 hexane is then evaporated under vacuum using a rotary evaporator, and then drawn off under vacuum for a further one hour after complete removal of the solvent. The extract obtained is then placed in an oven at 100'C. for 24 hours, and then analysed. 26 g of extract are obtained according to this method.
The physicochemical and chromatographic analyses of this extract gave the following results: incineration residue: <0.1% content of volatile compounds: <0.1% content of furanic lipids: 46% EXAMPLE 3 One kilogram of leaves of avocado plant of the Hass variety is carefully ground. The ground product is brought into contact, with stirring, for 5 hours, with liters of methanol, 10 liters of chloroform and 10 liters of salt water (containing 1% of NaCI). The mixture is then centrifuged and the solid pellet removed. The bottom liquid phase is recovered and then dried over Na 2
SO
4 The solvents are then evaporated under vacuum using a rotary evaporator, and then drawn off under vacuum for a further one hour after complete removal of the solvents. The extract obtained is then placed in an oven at 100 0 C for 24 hours, and then analysed. 21 g of extract are obtained according to this method.
004920303 6 The physicochemical and chromatographic analyses of this extract gave the following results: incineration residue: <0.1% Scontent of volatile compounds: <0.1% content of furanic lipids: 46% EXAMPLE 4 One kilogram of leaves of avocado plant of the Hass variety is carefully ground. The ground product is then dried in an oven, under a hot air stream, at 110°C for 24 hours. 302 g of dry matter are then recovered. The latter is then brought into 0 contact with 2 liters of hexane and then heated under reflux for 5 hours. Once cool, the mixture is filtered on a Buchner funnel and the cake is washed with three times 100 ml of hexane. The hexane is then evaporated under vacuum using a rotary evaporator, and then drawn off under vacuum for a further one hour after complete removal of the solvent. 31 g of extract are obtained according to this method.
The physicochemical and chromatographic analyses of this extract gave the following results: incineration residue: <0.1% content of volatile compounds: <0.1% content of furanic lipids: 41% EXAMPLE One kilogram of leaves of avocado plant of the Hass variety is carefully ground. The ground product is then dried in an oven, under a hot air stream, at 70 0 C for 72 hours. 315 g of dry matter are then recovered. The residual moisture present in the leaves is then This dehydrated material is then brought into contact with 2 liters of hexane and then heated under reflux for 5 hours. Once cool, the mixture is filtered on a Buchner funnel and the cake is washed with three times 100 ml of hexane. The hexane is then evaporated under vacuum using a rotary evaporator, and then drawn off under vacuum for a further one hour after complete removal of the solvent. The extract 004920303 7 obtained is then placed in an oven at 100'C for 24 hours, and then analysed. 23 g of extract are thus obtained according to this method.
The physicochemical and chromatographic analyses of this extract gave the following results: incineration residue: <0.1% content of volatile compounds: <0.1% content of furanic lipids: 38% COMPARATIVE EXAMPLE METHOD WITHOUT EXCESSIVE HEATING OF THE LEAVES Example: one kilogram of leaves of avocado plant of the Hass variety is carefully ground. The ground product is then dried in an oven, under a hot air stream, at for 96 hours. 307 g of dry matter are then recovered. The latter is then brought into contact with 2 liters of hexane and then heated under reflux for 5 hours. Once cool, the mixture is filtered on a Buchner funnel and the cake is washed with three times 100 ml of hexane. The hexane is then evaporated under vacuum using a rotary evaporator, at 60°C, and then drawn off under vacuum for a further one hour after complete removal of the solvent. 27 g of extract are obtained according to this method.
The physicochemical and chromatographic analyses of this extract gave the following results: incineration residue: <0.1% content of volatile compounds: <0.1% content of furanic lipids: 2% Conclusion: in the absence of extensive heating of the leaves, or of the plant extract obtained from the fresh or dehydrated leaves by a solvent extraction, the final extract obtained contains practically no furanic lipids (content considerably less than 005161596 7a 00 oO As used herein, except where the context requires otherwise, the term "comprise" and variations of the term, such as "comprising", "comprises" and "comprised", are not intended to exclude other additives, components, integers or steps.
Reference to any prior art in the specification is not, and should not be taken as, ,0 5 an acknowledgment, or any form of suggestion, that this prior art forms part of the 0 common general knowledge in Australia or any other jurisdiction or that this prior art c could reasonably be expected to be ascertained, understood and regarded as relevant 0 by a person skilled in the art.

Claims (18)

1. A method for producing a plant extract comprising 20 to 80% furanic Slipids, wherein the raw material consists of avocado leaves and the method comprising: \exposing leaves to a solvent in a liquid-solid extraction step followed by 01 5 evaporation under vacuum, and ICN 0a heat treatment step between 80°C. and 1200C. for a period of time, it being c possible for these two steps to be carried out in this order or in the reverse order.
2. The method of claim 1 for producing a plant extract comprising 20 to furanic lipids, wherein the avocado leaves are obtained from avocado plants belonging to the following varieties: Hass, Fuerte, Ettinger, Bacon, Nabal, Anaheim, Lula, Reed, Zutano, Queen, Criola Selva, Mexicana Canta, Region Dschang, Hall, Booth, Peterson, Collinson Red or Alpha Krome.
3. The method of claim 1 or 2 for producing a plant extract comprising to 80% furanic lipids, wherein the heat treatment is carried for a period varying between 5 and 72 hours.
4. The method according to any one of claims 1 to 3 for producing a plant extract comprising 20 to 80% furanic lipids, wherein the appropriate solvent or solvents during the liquid-solid extraction step are chosen from the group consisting of alkanes, halogenated alkanes, ethers, esters, alcohols, aromatic compounds and supercritical fluids. The method according to any one of claims 1 to 3 for producing a plant extract comprising 20 to 80% furanic lipids, wherein the appropriate solvent or solvents during the liquid-solid extraction step are selected from the group consisting of hexane, ethanol, methanol, chloroform, dichloromethane, and ethyl acetate, taken alone or in the form of a mixture. 005161596 00 9
6. A method for producing a plant extract comprising 20 to 80% furanic lipids, the method comprising: Step 1: dehydrating avocado leaves, Step 2: liquid-solid extracting of said avocado leaves using a solvent, ,O 5 Step 3: vacuum evaporating said solvent until a plant extract is obtained, 0 Step 4: heat treating said plant extract at a temperature between 80 0 C and q 120 0 C.
7. Plant extract of avocado leaves which is obtained by the method according to any one of claims 1 to
8. The method according to any one of claims 1 to 5 wherein said heat treating step is performed in the presence of an acid catalyst.
9. The method according to any one of claims 1 to 5 where said leaves are ground before any step in the described method is performed. The method of claim 6 where said dehydrating step is performed at a temperature that is less than or equal to
11. The method of claim 6 or 10 where said dehydrating step is stopped when the residual moisture reaches the level of
12. The method according to any one of claims 6, 10 or 11 where said leaves are ground before any step in the described method is performed.
13. The method according to any one of claims 6, 10, 11 or 12 where said heat treating step is performed in the presence of an acid catalyst.
14. The method according to any one of claims 6 or 10 to 13 for producing a plant extract comprising 20 to 80% furanic lipids, wherein the avocado leaves are obtained from avocado plants belonging to the following varieties: Hass, Fuerte, 00516159E 00 Ettinger, Bacon, Nabal, Anaheim, Lula, Reed, Zutano, Queen, Criola Selva, Mexicana S Canta, Region Dschang, Hall, Booth, Peterson, Collinson Red or Alpha Krome. The method according to any one of claims 6 or 10 to 14 for producing a plant extract comprising 20 to 80% furanic lipids, wherein the heat treatment is carried 3 for a period varying between 5 and 72 hours. N16. The method according to any one of claims 6 or 10 to 15 for producing a (Ni plant extract comprising 20 to 80% furanic lipids, wherein the appropriate solvent or Ssolvents during the liquid-solid extraction step are chosen from the group consisting of alkanes, halogenated alkanes, ethers, esters, alcohols, aromatic compounds and supercritical fluids.
17. The method according to any one of claims 6 or 10 to 15 for producing a plant extract comprising 20 to 80% furanic lipids, wherein the appropriate solvent or solvents during the liquid-solid extraction step are chosen from the group consisting of hexane, ethanol, methanol, chloroform, dichloromethane, and ethyl acetate, taken alone or in the form of a mixture.
18. The method according to any one of claims 6 or 10 to 17 for producing a plant extract comprising 20 to 80% furanic lipids, wherein the dehydration is selected from the group consisting of drying under a heated air stream, drying under a controlled atmosphere, drying at atmospheric pressure under vacuum, drying the avacado leaves in a layer, microwave drying, spray-drying, freeze-drying, and osmotic dehydration in solution and osmotic dehydration in solid phase.
19. The method according to any one of claims 6 or 10 to 17 for producing a plant extract comprising 20 to 80% furanic lipids, wherein the dehydration consists in drying the avocado leaves in ventilated dryers, in a layer of the avocado leaves and under a hot air stream, at a temperature between 70'C and Plant extract of avocado leaves which is obtained by the method according to according to any one of claims 6 or 10 to 19. S005161596 00 O (N \O O 5 ^D (N
21. A method according to claim 1, substantially as hereinbefore described with reference to any one of Examples 1 to
22. A method according to claim 6, substantially as hereinbefore described with reference to any one of Examples 1 to
23. A plant extract according to claims 7 or 20, substantially as hereinbefore described.
AU2003269064A 2002-07-30 2003-07-28 Method for producing an avocado leaf extract rich in furanic lipids Ceased AU2003269064C1 (en)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
US10/206,995 2002-07-30
FR02/09666 2002-07-30
FR0209666A FR2843027B1 (en) 2002-07-30 2002-07-30 PROCESS FOR OBTAINING AN EXTRACT OF AVOCADO LEAVES RICH IN FURNA LIPIDS
US10/206,995 US6733795B2 (en) 2002-07-30 2002-07-30 Method for producing an avocado leaf extract rich in furanic lipids
PCT/FR2003/002377 WO2004012752A2 (en) 2002-07-30 2003-07-28 Method for producing avocado leaves extract rich in furan lipids

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AU2003269064B2 AU2003269064B2 (en) 2008-06-05
AU2003269064C1 true AU2003269064C1 (en) 2009-01-08

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KR (1) KR100944059B1 (en)
AR (1) AR040738A1 (en)
AU (1) AU2003269064C1 (en)
BR (1) BRPI0313419B8 (en)
CA (1) CA2493981C (en)
DE (1) DE60317679T2 (en)
ES (1) ES2295624T3 (en)
IL (1) IL166568A0 (en)
MX (1) MXPA05001237A (en)
WO (1) WO2004012752A2 (en)
ZA (1) ZA200501528B (en)

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