`Of U.S. Patent 8,278,351
`Exhibit
`ENZYMOTEC - 1008
`
`Petition for Inter Partes Review
`Of U.S. Patent 8,278,351
`Exhibit
`ENZYMOTEC - 1008
`
`(cid:19)(cid:19)(cid:19)(cid:19)(cid:19)(cid:20)
`
`
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`000002
`(cid:19)(cid:19)(cid:19)(cid:19)(cid:19)(cid:21)
`
`AKER877ITC00068707
`
`
`
`1538300
`
`METKGD FOR THE PROCESSEEG G? KRILL
`
`ffl ERGDUCE PRQTEXN, bl?1&fi ANQ CHXTIN
`
`Th0 prafiant
`
`invention ralatmfi to mmthw§a for aha
`
`prwmaaaing a: kril} to graduae yrotein, 3ip€$s
`
`anfi chitin.
`
`Kri11 fig a pumayeutiva SOUEUQ of
`
`[wed Qrmfigin ané other
`
`practically usefu} mejantfi gush as chitin Gflfi lipida which
`
`find wide appiication in different branchea 0f ghe natimnal
`
`Damnomy *« tha £906 infiuatry, textile anfi paint and varnifih
`
`1Q
`
`inénatry,
`
`in agrimulture anfl medicine“
`
`Knmwn in thg firt 13 a mathmé ffir the prafiuchiun Of
`
`a protainacmaufi mmtxitive Subatancfi
`
`frwm krill rmaiding in
`
`camminuting and gregfiimg freah or frozwn and than defrosted
`
`krill.
`
`Th0 lfiquifi fiaparatwd fiuring greaging is haatefl far 10
`
`t0 15 minute& at a temgexatura of 90 t0 93°C far coagulation
`
`0f proteinS cantainfid thmrain.
`
`The prmfiainacamua ooagulata
`
`is fiaparated from tha hreth by filtraxiwn or éemtrifugatien
`
`to pradume a maag which :0 aged in tha U353 undez a trada name
`
`of tha Okean pratein pagta.
`
`A disadvantage of saia m0tho§ for the yrocwg5ing of
`
`krili i3 1000 mi nutxitivw aubatanmes, particuiaxly protein,
`
`and an insuffiaianaly fall utiliz&timn 0f mhhfir campvnants
`
`mf krill.
`
`Th0 brmth cafitaining a congfifiarablm amount of
`
`nutritiva 50b50$009$ is mat prmmaasad 00a 15 yaured off.
`
`The
`
`yield of protein is 35 :0 46%.
`
`It shdulé ha painted out that
`
`tha Okean paste is a perishable product and shauld bé storefl
`
`only when frazan at a temperature not exveefiing «13°C for not
`
`were than 12 ha 16 mumtkfl.
`
`Thw thexmalky flun$tured protein
`
`containefl
`
`in th& Gkflan wa$fim 9030033w$ law fumwtiwnal prapartiés
`
`{fmfimmfmrming ané gfilwfiwrming prsparfiiafi, a wat0ywhmlflinq
`
`capacity, 000.; which makafi 1&0 praceaaxag an& 000 aiffiicultw
`
`The cake formed after grassing comprising a portion of the starting
`
`26
`
`3%
`
`(cid:19)(cid:19)(cid:19)(cid:19)(cid:19)(cid:22)
`000003
`
`3&2::5
`
`AKER877ITC00068708
`
`
`
`108W
`
`lipidg ana chitin integumafitfi can at pxeagng ha
`pxwtcina,
`prmawfisad and ufigfi Quiy as faed meal.
`'
`
`Knmwn in the art is a method fox the yruduction 05
`
`a protein canaantxate {ram fruzen krill keg: aé a tempelatuxe
`
`GE v20”C camyrising dfifkflfitfiLiQn; comminuhian 0f krill,
`
`axflraction with i§0§r0pfinwl with aubsaquwat remaval of th&
`
`golvgnt, and fivying unéfir vacuum at ?$”C*
`
`Uaéng tfla preaamt mmhhad a prmmwinacaaus cancwnurata
`
`13 prmdummfl with a ganuamt cf pywtein Qf ViQ ha 7?5%,
`
`lipids
`
`10
`
`mi 0.3%,
`
`an& chitin of 5.8 to 6.4% (as calculateé for dxy
`
`gubatance)“
`
`Said methad bag the follawing fiisadvantagefi.
`
`@he uaa of organic galvant makes the prwdactivn more éifficult.
`
`In additimng the galvent itself and the proc§$9 far the removai
`
`therewf may flat&riarata the quality of {hm ptctein.
`
`Tha groteimw
`
`amewug cancemtrafie h$$ & Camparativmly law fimnt&nt 0f pxwtein
`
`and a high chitin wantmmt.
`
`It is an ijfict of the pzament
`
`invgntien to develop
`
`Such a methnd fmr the praeassing of krill whimh weuld make it
`
`p0$$ible ta prmduaa prmtain,
`
`lipida anfi chitin with a high
`
`yielfi and quality~
`
`The methnd f0:
`
`tha grocaasing krill he yrodnaa
`
`protein,
`
`lipida ané chitin, &ccording ta the invantion,
`
`i5
`
`characterizad in campriaing amulsificatimn 9f lipifis Gf krill
`
`in an aqueous mefiium: geparation of tha amulaimn of lipids
`
`fxom tha kxill mflagg alkalinw axtracfiion wf yrmtfiing from th&
`
`krill mA$$ at a yfi Q5 13 t0 12: Sflpflrfifiimfi mf
`
`tha protein
`
`axtrac: profiucefi
`
`frwm whifiin ihtfiguWfinQfi; geyaraaimn mf protfiin
`
`fxem Eh$ pKutain exfizact.
`
`30
`
`product with d canteflé 0f prmtein of up :0 93% by weight a&
`
`The inventiQn makes it poafiiblg ta Qbfiain a protein
`
`calculated for dry Eubstance.
`
`a¢$0rding t0 aha invantion,
`
`thw 51:3: staga 0f tha
`
`000004
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`
`AKER877ITC00068709
`
`
`
`103 3900
`
`processfing of krili p}ovid§5 for extractian of lipiés. This
`
`axaxaatian mf lipid$ 13 affimchqd by @mulxiiicahiwn aaihg
`
`Vfif100$ mwchniquafi suwh 3% int&nxive mtitr§ng in &§ &ppaxatu$
`
`with a Shifter, a: an ultraaunic method. Used as a medium
`
`in which emulgifiaaciwn fig candufitfid i3 w&aex mr ngmewus
`
`SUIutiOhfi of salts.
`
`To raéuce lassas of yr$tein in the procafis
`
`0f smulgificuLiaa {ha pH mfi
`
`the amuisifying medium anguld be
`
`maintainaé wihhin 6‘8 ta $.0.
`
`In @mulgifimatiwn 3ip§dfi aré
`
`Seyaratefi with a yialfl of up ta 9§% by weight.
`
`The eril mftex aaparation of ligida Lhfirwfrom is
`
`traated With an alkalina fialuhion with a QR GE 10 t0 12 fax
`
`fixtzaetion mi prwtainfi
`
`thayfifrom.
`
`A hwmwyhaaa ayatam is farmmfi
`
`meprising an mqummufiwalkaline fimlution cmat&ining yrctain,
`
`an& a aoiifi resiflua cantaining chitin intagumenta anfi uther
`
`insmlublm subatanaea.
`
`Tha aqueoua-alkalina Salutimn contaiming
`
`prwtfiin i5 aaparatad from the solifi rasidué by filtzahion Qr
`
`cantxifugfitiqn.
`
`?rwt$in ia separatwd from the xefimltant
`
`aquwwugmalkalina Hmlutimn by variaus mehfiaafi! Ear axample,
`
`by precipitatimn with alcahml or uitrafiltration; pfiacipitatimn
`
`in the ixmmimetric @Qint,
`
`fir
`
`thexmal coagmiazian‘
`
`The 1&0“
`
`aigatric pracipitatgan i3 carriad Gut by fwod acifia at a pH
`
`mi 4 to 5.
`
`& cardigfi, eafiily settling pramiyitate of protein 15
`
`farmed whisk i3 saparated and waahefi with 2 to 5 valumes 0f
`
`watar.
`
`Th& wafihafl preaipiana 15 firifid.
`
`fix a rafiult a prmduct
`
`i3 obtaineé wiLh a proteia cantent 9f up to Q5% by waight as
`
`aalculat&§ fax dry fiubst&nm%,
`
`$hus,
`
`the propogefi metheé far the processing of krill
`
`makes it Pfififiiblfi ta prafiuca such va1uable substanees a5 yxwtein,
`
`iiyifls &nfi whitin,
`
`The simplg technolOgy $36 the availability Of
`
`the
`
`rafiQfi§nt$ mafia maka aha wrwmwsa cammezmiakly profiitahla.
`
`Far a batter unfierstanding of the pregent inventign
`
`000005
`(cid:19)(cid:19)(cid:19)(cid:19)(cid:19)(cid:24)
`
`AKER877ITC0006871 0
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`
`20
`
`30
`
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`1688309
`
`mxamglufi gym yrmxcntwfl kalow.
`
`Examglfi
`
`I
`
`In an nygaxatug winh a mapaciuy mi 10 i pxwvidmd wixh
`
`a fitirrmx thmra is wkacafl
`
`1 kg at krill whimh x0 fiilwfl with
`
`water and 3tirxw0 4t 13000 rpm Emr 0.3 hmur.
`
`Th9 rwfiulfi&nt
`
`amulfiimn 0f iigicm i3 geparafimd frwm the krili mama by
`
`filtrafiimm fihxmmgh a gtximlwgfi gtwak garmmm having a magh 3iz&
`
`Qf lxi nm*
`
`Th0 kriil ma%$ 1% afian§fwnrwfl
`
`tw the Uflfififll with a
`
`fitirrer imtm whiwh fihaxw i3 &0d&& 3 l 05 an aquwwum aolufijmm
`
`10
`
`0f N03“ wfi aumh a mmwcwnmranimn a0 an ra0mh a pH mf
`
`thm mixturfi
`
`Qf £0 and Riéwid far half an hmur,
`
`thm Mai}:
`
`fig tremhfifl
`
`with alkali @xtraatign 0f prflkwin$ makwfi
`
`fllfififi.
`
`T00 rafimltamt
`
`axtraan mi yratflina ix fiaparanad frmm tha Amsmiubia Kwfiiflwfi mg
`
`cfiitim imtfigmmantfl my filtratimn bhramqh a m0tal Scrfien witfi a
`
`maah @130 mi lxl mm aha menfixifugmfi at 2§s000 fipm far 0.;5 hfiur
`
`aw rfimmva imfid§iiimmu
`
`Tm fine purifiiea fixtract 0f wrmtwfing tharfi
`
`1% $dfiafl Whiifi fiairring a
`
`immala fiolmtimm 0? “Ci ta saawh a $0
`
`wk &.5, prmfiain bfling prmmipifiatadfl
`
`The pfififlé§ififita £5 imit
`
`t0 fifihtifi far R hwura, ahflrwaiher it is gayarahwd frmm Chg liquia,
`
`w&&hmfi with 3
`
`Iitfififi mf watwr and firifid lymyfiixiga11yw ?h$
`
`prmtein prmfiuat mbtaiwafi
`
`im an ammmmt mfi 30 g £5 a galflwpink
`
`mfimrléaa @wwaexg having a mwiatura momtmmt $5 30% by waigha anfi
`
`00mpx1$iwg 35% by weighg<3£pxmtaimamuizz my Wright mi
`
`liyiaa.
`
`Tha $081000 01 krill yraflucafi affiflx fiagaratiwn mf
`
`thg wmtxact mi prateinfi
`
`i3 pxegaafl hm rawmvm mmiauura and dri@&
`
`ta graducm 1? g Qf whitin intagumfintfi,
`
`Examplfi
`
`2
`
`Thw prwfiafifiihg 0r kriii i5 maflrififi ant
`
`km the $fimm
`
`mannwr 03 in RmaM§La l, QMfifipfi that amul3ifimfitimn mi
`
`lxpififi
`
`30
`
`i3 magfimmtafi
`
`in a 001% mmla aqu$wu$ fifilmtian wf gwfiium
`
`ahlmrifia at 0 90 0f 00%“
`
`The prwnein pradumt mhtminafl
`
`in an
`
`ammuht of 58 g h0a a mai0curg mmnfianu 0f 3&3 anfi mamymiaag 00%
`
`my waight mf yxwtezm and “a by weight m£
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`itpzdfi, anfi 20 g Q?
`
`AKER877ITC00068711
`
`
`
`10963300
`
`vhitin inacgumamtg.
`
`wxamwima 3
`
`The pchcasing of krikl ia canducted in the same
`
`manner as in Example 1, except that amulsificatian of lipifia
`
`is carried out for half an haur, anfi protein is precipitatefi
`
`from the alkaline extract by adding thareto a 1 mole salufiian
`
`uf acetic acid.
`
`The resultant gratein prmoipitate is washed
`
`with 3 volumes of watfix ta pgmfimme $0 g of a pnmmmin prgduat
`
`having a moi$turm cmntgnt 0f 8% and ammyxiging 85% by waight
`
`10
`
`of pxotein,
`
`5% by waigh: Qf Eigifls and 18 9 GE Chitin intcgummnta.
`
`Examplu a
`
`The pxmuafising GE krili ig caxried out
`
`in thw fifimfi‘
`
`m§nnex as in Example 1, axamp: that yxecipitation 0f prmtein
`
`Exam the alkaline extract i3 canduatefi by adding therato a 0.8
`
`mala fiolution of sulfuxic aaia. Tha yesultant precipitata
`
`0f yrctein is washad with 3 valmmfia GE watér t0 produce 5a g
`
`@f a protain product having & maigtuxe acntant Of
`
`lL% anfi
`
`camyxising 80% by wcight 0f yrmtmin and 5% by weight of lifiififi;
`
`anfi 2& g 0f mhitin integumefitfi.
`
`Exampka 5
`
`The prOcesfiing OE Krill ia wonfiucted in tha same
`
`manna: as in Example 1, axcagt that amulsification sf ligxds
`
`i5 manamatad in an aqugmua aeluti$n 3f aalua "w 0.2 mola 0f Mac};
`
`0093 mwla 0f MgCl
`
`2;
`
`0.81 mwla mf MgfiQa; anfl 0.005 male mf Caaflé.
`
`The protmin prafiumt mhtainafi
`
`in an gmount 0f 50 g
`
`has a moifiturm mantant mi
`
`;0% anfl wnmprifieg 82% by waiqha mt
`
`pxmmein, 4.2% by wwigh: 0f lipiflfif &mfl 20 g of chitin ifltfigumfintfi.
`
`39
`
`000007
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`
`AKER877ITC0006871 2
`
`
`
`liguia, waahefi witn 5 litams of water &afi driefi
`
`lyophilim
`
`3&l1y. Que pretain pxa&u$t obtainaa in an amennt of $0 g
`
`1E a palewpink adoslgss gowfler, having a woisbute centent
`
`of 30% by weight and camgriging 85% by waigfifi Sf yrotein
`
`gné 2% by waight 0f ligiés.
`krEfi
`@ha raaidue 0ftkw&eé produced afitcr xaparation uf
`
`tag fixtxact of profieima :3 preaaed to rgmova moisture aaé
`
`daied to praauue l? g cf chitin intagumaafifi.
`
`)
`Example 2
`Que proeaafiing 9f-égig& is carriefi eat in the flame
`
`magma? as in Example l, except that emuiaifimabion of ii»
`
`piéa 13 conductfid in a 0.1fi mole aguaous fiwlution ofi Sodium
`
`saloxfiaa at a fifl 0g &.§. The prutain profluct thainaa iu
`
`fifl amfiunt of 54 g baa & moisbura content 9f 12% and campriS»
`
`as 80% by weight of pratein and §% by waigmfi of lipida, anfi
`
`20 g af chitin intagumenta.
`
`;
`
`.
`
`\k
`
`Examyla 5
`
`ri/i
`fine procfisaing af.ky&gi~is conductad im the game man—
`
`may aa in Example 3, except that emulaifiicafiion cf lipidfi
`
`is sarried out fior half an hour, and grotaiu is pxeaipitaw
`
`tea from the alkaliaa %xCract by adding thereto a 1 mole
`
`afiiutinn ofl asatic acid* ?he resultant grotain precipitate
`
`is wafihéfi wifih S vakumes 0f water to prefiuca 60 g of a prom
`
`fiaia product having a maisture content of 8% &ufi comprialag
`
`&5% by weight of prfltain, §% by weight 0f lipids and 18 g
`
`000008 N
`(cid:19)(cid:19)(cid:19)(cid:19)(cid:19)(cid:27)
`
`AKER877ITC0006871 3
`
`
`
`
`
`1038900
`
`o£ chitia intagumentau
`
`.
`Examplw Q
`wne yxacaaaing a£~éggi% i3 agrriea out in fine same
`
`manner as in Example 1, excepfi that precipitafiion Qf pro-
`
`tain £39m the alkaline extract is aoaémated by adding fiberaw
`
`ha a 0.8 mola solution of sulfuria aaifi. The resultant pra—
`
`cipitata Qf pratain is waal’wé} with ,7: valumes of avatar“ to
`
`produca 54 g 93 a ywotein praduct having a moisture mgatnnt
`
`0f 11% ané compxifiing 80% by waight 0f grobein and 5% by
`
`weight 0f Kipififi, an& 34 g of chitin infiegumanha.
`
`Wamyla 5
`
`(«HI
`The yraaessing ofmk%é@% is canflacted in the sama
`
`manna: as in Example 1, exae§t fiaat emulsifioation of li~
`
`pids is caaauctefi in an aquagux salufiimn of salta mu 0.2 mole
`
`of Racl; 0‘05 mole of MgClzg 0.01 maia 0f M3804; and 0.005
`
`mole 0f CaSQQ.
`
`Thfi pretain product obtainad $3 an amount of 60 g
`
`flag a moistura snutent of 10% an& $Qmprisea 82% by wgight
`
`of protaing 4,2% by weight of lipids, anfi 20 g 0f chitfiu
`
`integamaata.
`
`000009
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`
`AKER877ITC00068714
`
`
`
`10989400
`
`wua EMRQwENEN?fi OF THK INVER?EQN 3N WHICH AN EXCLU$EVE
`
`PROPERTY OR 0RXVELEGH {S CLAIMHB ARE BEFEREB £3 FOLLOQS:
`
`l.
`
`A mehhofi for the processing Sf krill to Produce
`
`protein, lipids and chitin which comprises emulaitication or
`
`ligids of krill in an aqucaua mediUm; gepaxatian of
`
`the
`
`msmnxmt emulsion of lipic‘m {from mm mm mama; alkaline:
`
`axtrachion 0f prmtaina gram the krili mgmg at a pH Qf 10 to 12;
`
`5e9afi§pimn Q5 tha aikaline gxtract 55 pretains fismm chitin
`
`integumanha; aaparatimn of protain frmm thfi alkalina extract.
`
`2“
`
`A methoé as Claimgd in alaim 1, wherein emulsifii~
`
`fiatien is carried Qut in tha prasenca mf minaral $alts.
`
`?,- A mathmé a3 claimefi
`
`in ciaim 1, wherein emulaifiw
`
`cation fifi cartiaa amt at a pH of hhe medium $5 4.5 t0 5.0.
`
`0000010
`(cid:19)(cid:19)(cid:19)(cid:19)(cid:19)(cid:20)(cid:19)
`
`AKER877ITC0006871 5
`
`
`
`SUBSTITUTE
`
`REMPLA CEMENT
`
`SECTION is not Present
`
`Cette Section est Absente
`
`0000011
`(cid:19)(cid:19)(cid:19)(cid:19)(cid:19)(cid:20)(cid:20)
`
`AKER877ITC0006871 6
`
`