(12) United States Patent
`Beaudoin et al.
`
`US006521768B2
`(10) Patent N0.:
`US 6,521,768 B2
`(45) Date of Patent:
`Feb. 18, 2003
`
`(54) PROCESS FOR THE EXTRACTION 0F
`LIPIDS FROM FATTY BIRD TISSUES
`
`(51) Int. C1.7 ................................................ .. C07C 1/00
`(52) us. Cl. .................................... .. 554/14; 8/12; 8/13
`
`(76) Inventors: Adrien Beaudoin, 748, boul des
`Vétérans, Rock Forest, Quebec (CA),
`J 1N 1Z7; Genevieve Martin, 660, Cote
`Ste-Genevieve #2, Quebec, Quebec
`(CA), G1R 3K5
`
`( * ) Notice:
`
`Subject to any disclaimer, the term of this
`patent is extended or adjusted under 35
`U.S.C. 154(b) by 0 days.
`
`(21) Appl. No.: 10/037,086
`.
`_
`(22) Flled'
`(65)
`
`NOV‘ 9’ 2001
`Prior Publication Data
`Us 2002/0133033 A1 56p‘ 19 2002
`
`(30)
`
`Foreign Application Priority Data
`
`(58) Field of Search .............................. .. 554/8, 12, 13,
`554/14
`
`Primary Examiner—Deborah D. Carr
`74 Attorne , A em, or Firm—Eric Fincham
`(
`)
`y g
`(57)
`
`ABSTRACT
`
`A method for the extraction of lipids from lipid containing
`tissues of a member of the bird species such as the ratite,
`gallinaceous or anatidae Wherein the lipid containing tissues
`are comminuted and the lipids extracted in a solvent, pref
`erably acetone or ethyl acetate, to provide a liquid fraction
`and a solid fraction and subsequently removing the solvent
`from the liquid fraction to provide a lipid rich component.
`
`Nov. 14, 2000
`
`(CA) ........................................... .. 2325377
`
`9 Claims, No Drawings
`
`NEPN Ex. 2042
`Aker v. Neptune
`IPR2014-00003
`
`Page 1
`
`

`
`US 6,521,768 B2
`
`1
`PROCESS FOR THE EXTRACTION OF
`LIPIDS FROM FATTY BIRD TISSUES
`
`This present invention relates to a method for the recov
`ery of lipids from bird tissues.
`Birds possess varying amounts of fat tissue under their
`skin and in their peritoneal cavity. The recovery of the oil or
`lipids from the lipid containing tissues of birds is desirable
`for various uses such as a nutriment, nutraceutical or cos
`metic.
`The knoWn methods for recovering lipids from lipid
`containing tissues of birds usually comprises the heating of
`the lipid containing tissues once they have been removed
`from the bird.
`In general, the fatty tissues from birds Which are raised
`for food purposes are collected in slaughterhouses. Today,
`fat in generally has a bad reputation and accordingly it is
`frequently considered as Waste or a loW value product. This
`reputation derives in part from the fact that the fats are often
`contaminated by bacteria such as salmonella. Accordingly,
`often the fats are frequently subjected to a heat treatment and
`at a relatively high temperature to destroy any bacteria. This
`results in oxidation of the unsaturated lipids.
`Certain oils derived from certain birds are considered to
`have a higher value. Thus, emu oil is taught in the art to have
`certain desirable characteristics. One desirable characteristic
`of emu oil is that it is particularly loW in cholesterol.
`It is an object of the present invention to provide a
`method for the extraction of lipids from lipid containing
`tissues of birds and Which preserves the quality of the lipids.
`According to one aspect of the present invention, there is
`provided a method for the extraction of lipids from lipid
`containing tissues of a member of the bird species, the
`method comprising the steps of comminuting the lipid
`containing tissues, placing the comminuted lipid containing
`tissues in a solvent for a period of time sufficient for at least
`a portion of the lipids in the lipid containing tissue to
`dissolve in the solvent to thereby provide a liquid fraction
`and a solid fraction, separating the liquid fraction from the
`solid fraction, and removing the solvent from the liquid
`fraction to thereby recover a lipid rich component.
`The method of the present invention may be applied to
`lipid containing tissues of any bird from Which it is desirable
`to recover high quality lipids. Particularly preferred are
`methods supplied Wherein the bird is a ratite, a gallinaceous
`bird or an anatidae (duck and geese family). Ratites include
`the emu, nandou, and ostrich, all of Which have had oils used
`for their health bene?ts by aboriginals in Asia, Africa and
`South America.
`As practiced commercially, the bird Would be bled prop
`erly and the fat removed and cooled. Typically, the fat may
`be froZen to facilitate the handling of the tissue.
`The step for comminuting the lipid containing tissues
`may be carried out by any conventional means. Thus, one
`Would process the tissues at ambient temperatures. The
`tissues may be comminuted by means of a grinder or other
`suitable means.
`The comminuted lipid containing tissues Would then be
`subjected to extraction using a suitable solvent. Particularly
`preferred are acetone and ethyl acetate. The extraction
`Would be done at a relatively loW temperature and preferably
`betWeen 4° C. and 25° C. The temperature is not a critical
`parameter; a higher temperature Will increase the ambient
`level of the vapors of the solvent.
`The volume/Weight ratio of solvent to the lipid contain
`ing tissues may vary. Generally, the solvent tissue volume/
`Weight ratio should be at least 3:1 and a preferred ratio is
`betWeen 3:1 and 9:1.
`
`2
`Preferably, the solvent tissue mixture is agitated and any
`suitable means may be employed—a container equipped
`With agitation paddles as is Well knoWn in the art Will ensure
`an efficient mixing.
`The extraction time period may vary; generally, a period
`of time greater than 20 minutes has been found to be
`required.
`Following, the extraction, the liquid fraction and solid
`fraction need to be separated. Again, many apparati are
`knoWn in the art and to this end, one may use an apparatus
`for centrifuge. Alternatively, ?ltration could be utiliZed and
`in some instances, a combination of the methods can be
`appropriate—i.e. an initial centrifuge folloWed by a ?ltra
`tion. It Would also be possible, Where time is not a factor, to
`utiliZe sedimentation.
`FolloWing the separation of the liquid fraction and the
`solid fraction, the solvent Will be removed to provide a lipid
`rich component. The solvent may be removed by knoWn
`methods, including, for example, ?ash evaporation, straight
`evaporation or spray drying. The step may be practiced
`either in batches or on a continuous basis. The temperature
`can be increased up to approximately 125° C. for a very
`limited period of time. This Will ensure the steriliZation of
`the oils and during a limited period of time, Will minimiZe
`chemical changes in the lipids. To minimiZe oxidation, one
`could perform the step in a nitrogen atmosphere.
`Optionally, one can add an antioxidant to the liquid
`fraction to minimiZe lipid oxidation. Alternatively, the anti
`oxidant could be added after removal of the solvent. Still
`further, an antioxidant could be added during the extraction
`step. Any number of food grade antioxidants are knoWn in
`the art.
`Optionally, after separating the liquid fraction and the
`solid fraction, one may Wash the solid fraction With a
`solvent.
`Having thus generally described the invention, the fol
`loWing examples illustrate embodiments of the invention.
`EXAMPLE 1
`Lipid containing tissues from an emu Were subjected to an
`extraction process Wherein the extraction time and the
`solvent Were varied as set forth in Table 1.
`
`TABLE 1
`
`Standardization of the extraction process With emu fat.
`
`Solvent
`
`Vol/Weight
`
`Grinding
`
`acetone
`ethanol (21“)
`acetone
`acetone
`acetone
`acetone
`acetone
`ethyl acetate
`ethyl acetate
`ethyl acetate
`Chlor:MeOH**
`Chlor:MeOH
`
`9:1
`4:1
`9:1
`9:1
`9:1
`9:1
`9:1
`9:1
`9:1
`9:1
`10:1
`10:1
`
`—
`_
`—
`—
`yes
`yes
`yes
`yes
`yes
`yes
`yes
`yes
`
`Time
`(hours)
`
`20
`1
`18
`18
`18
`18
`30 min
`18
`30 min
`30 min
`30 min
`30 min
`
`Yield
`%
`
`37.5
`2.6
`39.6
`45.8
`*61.6
`75.4
`38.2
`87.6
`85.9
`87.4
`78.5
`80.0
`
`Experiments Were carried out in triplicate and variations between repli
`cates Were inferior to 5% of the highest value.
`Experiments Were carried out at 4° C.
`Lipids Were estimated by gravimetry.
`*Presence of skin With adipose tissues.
`**The method of Folch et al. (1957).
`
`10
`
`15
`
`20
`
`25
`
`30
`
`35
`
`40
`
`45
`
`50
`
`55
`
`60
`
`65
`
`EXAMPLE 2
`Lipid containing tissues of chicken Were then subject to
`extraction as set forth in Table 2.
`
`Page 2
`
`

`
`3
`
`TABLE 2
`
`US 6,521,768 B2
`
`4
`
`TABLE 4-continued
`
`Extraction of chicken fat
`
`Analysis of emu oil comparison With commercial re?ned oil
`
`Solvent
`
`vol/Weight
`
`Yield %
`
`acetone
`acetone
`ethyl acetate
`ethyl acetate
`
`9:1
`9:1
`9:1
`9:1
`
`9.8
`12.5
`*42.2
`60.9
`
`Experiments Were carried out in triplicate. Variations betWeen replicates
`Were inferior to 5% of the highest value.
`The extraction Was performed at 4° C., for tWo hours.
`Lipids Were estimated by gravimetry.
`*Presence of skin mixed With adipose tissues.
`
`EXAMPLE 3
`In this example, freshly ground lipid containing tissue
`from Peking duck Was immersed in 1/5 of their Weight of
`distilled Water at a temperature of 65° C. and gently agitated
`for 30 minutes While maintaining the temperature constant.
`Fat Was then separated from the solid and aqueous base by
`centrifuge. Volatile matter Was eliminated by heating for 30
`minutes at 130° C. under a nitrogen atmosphere. The yield
`of lipids as measured by gravimetry Was 50.6%. The experi
`ment Was carried out in triplicate.
`
`EXAMPLE 4
`
`The lipid containing tissues of the Peking duck of
`Example 3 Were mixed in a volume/Weight ratio of 5:1 With
`ethyl acetate and Were agitated gently for 30 minutes. The
`solvent Was evaporated and the lipids measured by gravim
`etry. The yield Was 67.5%.
`The experiment Was repeated With volume/Weight ratios
`of 3:1 and 9:1 and approximately the same results Were
`achieved.
`
`EXAMPLE 5
`
`The method of Folch et al, as previously discussed, Was
`carried out on the same Peking duck tissue. Ayield of 49.9%
`Was achieved.
`The lipids recovered in Example 4 Were then analyzed
`and compared With a commercially re?ned oil commercially
`available from Dundee Co. The analysis is set forth in Table
`4.
`
`TABLE 4
`
`Analysis of emu oil comparison With commercial re?ned oil
`
`Speci?cations
`
`Humidity
`Peroxide value
`Free fatty acids
`Refractive index
`Iodine values
`
`Beaudoin
`Martin
`
`<0.05%
`4.0-4.4
`0.18
`1,455
`67-89
`
`Commercial
`
`<0.05%
`<10
`<1.5
`1,456—1,467
`65-85
`
`10
`
`15
`
`20
`
`25
`
`30
`
`35
`
`40
`
`50
`
`55
`
`Speci?cations
`
`Saponi?cation values
`Speci?c gravity
`Microbiology col./ml
`Cholesterol (%)
`
`Beaudoin
`Martin
`
`195-212
`0.909
`<10
`0.04
`
`Commercial
`
`190-200
`0.897—0.920
`<10
`—
`
`Properties of emu oil are comparable to those of the
`re?ned oil on the market (Dundee Co). Criteria for comes
`tibility of the AOCS are met.
`We claim:
`1. A method for the extraction of lipids from lipid con
`taining tissue of a member of the bird species, said method
`comprising the steps of:
`comminuting said lipid containing tissues;
`placing said comminuted lipid containing tissue in a
`solvent for a period of time suf?cient for at least a
`portion of said lipids in said lipid containing tissue to
`dissolve in said solvent to thereby provide a liquid
`fraction and a solid fraction;
`separating said liquid fraction from said solid fraction;
`and
`removing said solvent from said liquid fraction to thereby
`recover a lipid rich component.
`2. The method of claim 1 Wherein said step of adding said
`solvent to said comminuted tissue comprises the step of
`adding a solvent selected from a group consisting of acetone
`and ethyl acetate.
`3. The method of claim 2 Wherein said member of the bird
`species is a ratite, a gallinaceous bird or an anatidae.
`4. The method of claim 2 Wherein said solvent is added to
`said comminuted fat containing tissue in a volume/Weight
`ratio of at least 4:1.
`5. The method of claim 2 Wherein said solvent is added to
`said comminuted tissue in a ratio of between 4:1 and 15:1.
`6. The method of claim 1 Wherein said solvent is added to
`said comminuted tissue at a temperature of between 0° C.
`and 25° C. and maintained at said temperature range for said
`period of time.
`7. The method of claim 1 Wherein said step of removing
`said solvent comprises a step selected from the group
`consisting of ?ash evaporation, evaporation and spray dry
`ing.
`8. The method of claim 1 Wherein the step of separating
`said liquid fraction from said solid fraction comprises the
`step selected from the group consisting of ?ltration, cen
`trifugal separation, and sedimentation.
`9. The method of claim 1 further including the step of
`Washing said solid fraction With a solvent prior to recovering
`said lipid rich component.
`
`Page 3