CS217423B1 - Method of izolating ergot alkaloids from cultivation suspensions - Google Patents

Method of izolating ergot alkaloids from cultivation suspensions Download PDF

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Publication number
CS217423B1
CS217423B1 CS787736A CS773678A CS217423B1 CS 217423 B1 CS217423 B1 CS 217423B1 CS 787736 A CS787736 A CS 787736A CS 773678 A CS773678 A CS 773678A CS 217423 B1 CS217423 B1 CS 217423B1
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CS
Czechoslovakia
Prior art keywords
adsorbent
mixed
swelling
process according
iso iso
Prior art date
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CS787736A
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English (en)
Inventor
Werner Grawert
Brigitte Neumann
Ludwig Schiedt
Karl-Heinz Heidenbluth
Christoph Dauth
Rudolf Schirutschke
Monika Muller
Original Assignee
Werner Grawert
Brigitte Neumann
Ludwig Schiedt
Heidenbluth Karl Heinz
Christoph Dauth
Rudolf Schirutschke
Monika Muller
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Application filed by Werner Grawert, Brigitte Neumann, Ludwig Schiedt, Heidenbluth Karl Heinz, Christoph Dauth, Rudolf Schirutschke, Monika Muller filed Critical Werner Grawert
Publication of CS217423B1 publication Critical patent/CS217423B1/cs

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D457/00—Heterocyclic compounds containing indolo [4, 3-f, g] quinoline ring systems, e.g. derivatives of ergoline, of the formula:, e.g. lysergic acid
    • C07D457/04—Heterocyclic compounds containing indolo [4, 3-f, g] quinoline ring systems, e.g. derivatives of ergoline, of the formula:, e.g. lysergic acid with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 8
    • C07D457/06—Lysergic acid amides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B60—VEHICLES IN GENERAL
    • B60M—POWER SUPPLY LINES, AND DEVICES ALONG RAILS, FOR ELECTRICALLY- PROPELLED VEHICLES
    • B60M1/00—Power supply lines for contact with collector on vehicle
    • B60M1/12—Trolley lines; Accessories therefor
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D519/00—Heterocyclic compounds containing more than one system of two or more relevant hetero rings condensed among themselves or condensed with a common carbocyclic ring system not provided for in groups C07D453/00 or C07D455/00
    • C07D519/02—Ergot alkaloids of the cyclic peptide type
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P17/00—Preparation of heterocyclic carbon compounds with only O, N, S, Se or Te as ring hetero atoms
    • C12P17/18—Preparation of heterocyclic carbon compounds with only O, N, S, Se or Te as ring hetero atoms containing at least two hetero rings condensed among themselves or condensed with a common carbocyclic ring system, e.g. rifamycin
    • C12P17/182—Heterocyclic compounds containing nitrogen atoms as the only ring heteroatoms in the condensed system
    • C12P17/183—Heterocyclic compounds containing nitrogen atoms as the only ring heteroatoms in the condensed system containing an indolo[4,3-F,G]quinoleine nucleus, e.g. compound containing the lysergic acid nucleus as well as the dimeric ergot nucleus
    • H—ELECTRICITY
    • H02—GENERATION; CONVERSION OR DISTRIBUTION OF ELECTRIC POWER
    • H02G—INSTALLATION OF ELECTRIC CABLES OR LINES, OR OF COMBINED OPTICAL AND ELECTRIC CABLES OR LINES
    • H02G1/00—Methods or apparatus specially adapted for installing, maintaining, repairing or dismantling electric cables or lines
    • H02G1/02—Methods or apparatus specially adapted for installing, maintaining, repairing or dismantling electric cables or lines for overhead lines or cables
    • H02G1/04—Methods or apparatus specially adapted for installing, maintaining, repairing or dismantling electric cables or lines for overhead lines or cables for mounting or stretching

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  • Organic Chemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Zoology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Health & Medical Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Biotechnology (AREA)
  • Genetics & Genomics (AREA)
  • Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • General Engineering & Computer Science (AREA)
  • Microbiology (AREA)
  • Mechanical Engineering (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Compounds Of Unknown Constitution (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Nitrogen Condensed Heterocyclic Rings (AREA)
  • Nitrogen And Oxygen Or Sulfur-Condensed Heterocyclic Ring Systems (AREA)
  • Indole Compounds (AREA)

Description

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HajiHqHH b οπθκτρθ pacTBopHMux b Boae qacTea, cHa^aaa nepe-MeuiMBaioT b TeqeHne okojio 30 mhh c 4-5 Bec.% (ο^μτθη HaoOseM yposaa) rjiHH03eua, cnocoÓHoro κ HaóyxaHHio, π pa3ae-jihiot uexaHHHecKH, HanpuMep, $HjiBTpoBaHneM, TBepaue κ sKa-κηθ $a3U. ílojiy^eHHtifó BjiaMNft MimejiHň nu cuecL BJiaxHuttΜΗΗβοβ-aflcopÓeHT cymaT b nceBaoooKOHHOu caoe řípu 80 -90 °C b τβ^θΗΜθ 20-40 mhh ao TeunepaTypu OTxoaninero bo3-ayxa OT 50 ao 70 °C h ao οοτθτοηηοΚ bji32khocth uaKCHuaaBHO15 %. Cyxoft uHiíejiuft um cueci cyxoft uHaeaiift-aacopóeHT npaHeoóxoaHMOCTH nocne pacTHpaHHH b nacTy c BoaHuu cjiaOoae-jioqHLiM pacTBopoM, Hanpnuep, 15 %-HOii auuHa^Hoíi Boaott,noaBepraiOT 3κοτρ3κηηη c anpoTOHHbiu opraHoecKHM pacTBOpn-Tejieu, HanpHuep, hk3iuhm 3$npoM aaKHJiKapOoHOBOií kmcjiotu,aneTOHOu hjih raaoreHHpoBaHHuu yraeBoaopoaou, nojiyqeHHUííOKCTpaKT b cay^ae HaoóxoauMOCTH aJin yaaaeHHH ηθοοηοβημχÓaaaacTHhix BemecTB noaaioT Ha oaKOCTHO-oaKOCTHyx) οκοτροκ—HHID C BOaHO-KMCJlOfí $a30ÍÍ B OÓBQUHOU COOTHOUieHMH 2:1 aO1:1. BoaHnfi, coaepjsaaHfí Bce ajiKajionau, pacTBOp nocjie noa-mejia^HBaHHH ao 3Ha*íeHHH pH b npeaexax 8-9,5 pesKCTparn-pymT opraHoecKHM HecueuiUBawiucH c Boaoft pacTBopuTejieu,npenuymecTBeHHO 3THJiau,eTaT0u, b οοοτηοιηθημη 1:1 ao 3:1.flaaHeftmafl nepepaÓOTKa npeaBapHTejiBHO οημιηθηηογο sKCTpaKTaocymecTBJíneTCH η3βθοτηειμ cnocoóou, πρηηημθη bo BHwuaHHexHMHHecKHe h £n3MqecKne cBOňcTBa cooTBeTCTByioinHx ajiKaaon-aoB. 3 ΠΡΚΜΕΡΗ ZCnOZHEHHfl
IlpzMep I 200 ji KyjiLTypaJiiHOít cycneH3ZZ nraaMMa Claviceps purpurea(Fr.)Tul. IL3T PA13O(xpaHHTCfl B UeHTpaJIBHOM ZHCTZTyTOMHKpodzojiorzz z sKcnepzMeHTajiBHoM TepanzH, iíeaa) nepeMQ-nMBaioT 30 mhh c 8 κγ óeflTOHHTa z 3aTeu $zjiBTpyioT nepe3Bpamawiíícfl HnozcTtifí BaKyyM—$hjibtp c 10 mm-bhm cjioeM H3azrzapaTa cepHOKHCJioro KajiBííHH. OzjiBTpaT, πρέκτζ^βοκζcboÓoíhhíí οχ aJiKaJiozAOB, BHÓpacfciBaioT; CHHTyio ομθοβ BJias-ΗΗϋ ΜΗΙίβΗΗϋ-όβΗΤΟΗΗΤ CyiIiaT B ΠΟΘΒ,ζΟΟΗΖΚΘΗΗΟΜ CJIOe npzTeMnepaTypo πρζτοΉΐΟΓο B03syxa 90 °C ao τθχ nop, noxa τθμnepaTypa OTxoflHinero B03syxa ηθ λοοτηγηθτ 60 °C (npo^oji-szTejiBHOCTB okojio 30 mhh). IIojiy^aioT 20 βθ 24 κγ CMecz cy-XOfl MZIieJIHÍt-ΟβΗΤΟΗΗΤ C OCTaTO^HOfí BJiaSHOCTBIO 3-5%, KOTO-pas coflepxHT 95-100% sproTOKCZHa, onpeaejieHHóro b KyjiBTy—pajiBHOtt cycneH3ZH, z 92-96% sproMěTpzHa. ΠρΗΜβρ 2 · ' 100 ji KyjiBTypaJiBHoK cycneH3ZZ, yKasaHHoro b npzMepe IDiTauMa Claviceps purpurea nepeMeinzBaiOT b TeneHze Inaca c 5 κγ OTóejioaiouíeíí rjiZHH, $zjiBTpyioT z ομθοβ BJiaacHNÍÍMziíejizň-OT(5ejizBaiomafl rjizHa cyniaT b nceBflooszaceHHOM cjioeb τθηθηζθ 15 mzh npz 80-90 °C ao TOMnepaTypu οτχοαηχθγοBO3Ayxa 50 °C. IIojiyqaioT 12 κγ ομθοη cyxoft Mzuejizft-OTÓejiz-Baioinafl rjizHa c ocTaTOHHOíí BJiaaHOCTBio 10-12% z co^epsaHzeuaJiKajiozaa 92-100%, cqzTan Ha KyjiBTypaJiBHyw cycneH3Zio. Πρζΐίβρ 3 10 κγ npzroTOBJíeHHOit no npzidepy I zjiz 2 CMecz cyxofíliznojizfí-aTicopÓeHT 3aMemzBamT c 1,5 ji pa3tfaBJieHH0ií 1:2asíMza^Hon bojuj, nocjie 5-10 mzh HatfyxaHZH neperemzBaiOT c40 ji sTZJiaqeTaTa b 2 nopuznx no 15 mhh c uitra-Turraxz OTcacuBaioT; oóqzM οκοτροκτ βμθοτθ c 20 ji 3%-hoK boahoíí 4 φοοφορΗΟϋ khcaoth nponycKaioT nepe3 cenapaTop. K THsenořiφθ3θ npudaBJíHiOT 8 ji 3ToaiieTaTa, npn nepeMemiiBaHim ycTa-Η3ΒΑΗΒ3Κ)Τ pH Ha 8,5 AO 9,0<| AOÓaBAHH KOHUeHTpHpOBaHHyiOaMMua^Hy» BOAy h 10 mhh nepemeuiMBaioT. Tlocjie pa3A0ASHHHφ83 noBTopfiioT c 6-8 sTHjiaueiaia ema 2 pasa. OOamíí sKCTpaiíKOHiieHTpupyioT ao 0,3-0,6 ji b BaKyyMHOM ιιηρ^αηημοηηομ kc-napiiTejie, b ββιπθρηομ annapaTe c hhcxoahiw ποτοκομ yna-pHBaeMOÍÍ XHAKOCTH MAM APyr^M ΜΗΓΚΜΜ ΜβΤΟΑΟΜ ynapKH, CMe-ΙΠίΙΒ3Κ)Τ c aboKhhm ΟόΒΘΜΟΜ ΧΑΟρΟφΟρωθ Η ΟΤΑβΑΗΙΟΤ aprOláeTpHHΒ φθρΜ6 TpyAHOpaCTBOpHMOrO ΧΑΟρΟφΟρΜΗΟΓΟ aAAyKTa. ΡΙ3φΗΑΒτρ3Τ3 nonynaiOT nocne οπμοτκη aACopÚiiMOHHOií xpowaTO-ΓρθφΗθίί ΚΟΑΟΗΗΗΜ ΜΑΗ ΠβρΗΟΑΜΗβΟΚΜΜ ΟΠΟΟΟ0ΟΜ aprOTOKCMH ΒΒΠΑθ 0θΗ30ΑΒΗ0Γ0 ΜΑΗ TOAyOABHOrO aAAyKTa.
Oda aAAyKTa οίμαθημ tohkocaoííhoíí xpoMaTorpaíneft η οοΑθρ-acaT ot 96 ao 103% aAKaAOHAa b pacneie Ha 0ΗΜ3ΑβΗΗ3τ· Bu-xoa cocTaBAH6T 58,6 r aproTOKCMH—TOAyoA—aAAyKTa = 72%' bpacqeie Ha KyABTypaABHyio cycneH3Hio h 40,5 r sproueTpHH -χΑοροφορω-aAAyKTa = 82% b pacneTe Ha KyABTypaABHyio cyc-Π6Η3ΗΚ)< ΠρΗΜδρ 4 60 κτ noAyneHHOií no npHMepy I mam 2 cmsch cyxoň μμιιθαηΚ-aAcoptfeHT 3aueniHBaioT c 7,5 a pa3óaBA6HH0íí 1:1 aMMHanHofóboah, BKCTparMpyioT b sKCTpaKTope c MeinaAKOft 150 a xAOpo-φθρΜ3 MAM XAOpHCTOrO ΜβΤΗΑΜΟΒ Τθ^θΗΗΘ 45 MMH, SKCTpaKTφHABTpyíOT ΠΟΑ ΑΟΒΑβΗΗΘΜ H 3KCTpaKIJHI0 ΠΟΒΤΟρΗΙΟΤ C ΤΘΜ seΟύΈΘΜΟΜ paCTBOpMTSAfl Β ΤβΠβΗΗΘ 30 ΜΗΗ. OÓahíí aKCTpaKT nponycKaioT nepe3 cenapaTop c 5%-hoK boa-HOÍt BHHHOÍl ΚΗΟΑΟΤΟϋ Β ΟΟΟΤΗΟΠΙΘΗΗΗ Iíl, BOAHyiO φa3y ΗΘΠρθ-puBHO ycTaHaBAHBaioT Ha pfí 9 h canapHpyioT Βτοροίί pa3 c τθμse pacTBopHTeAeM mam c βτηαθπ,θτθτομ β οοοτηοπιθημμ 2:1.ΠΟΟΑθ BHnapHBaHHH, ΟΤΑθΑΘΗΗΗ 3ρΓ0ΜΘΤρΗΗ3 Η ΟΟΘΧΑθΗΗΗ 3ρΓ0-TOKCHHa nojiynaiDT aAAyKTa c buxoaom μ κβηθοτβομ, yKa3aHHtiMb npMMepe 3. 5 ΠρκΜθρ 5 30 ji KyjiLTypaJiLHOro pacTBopa, o<5pa3yioinaro apro3MH iniaMuaClaviceps purpurea BIST PA 134, nopeueiUMBaiOT πρπ eCTeCT-B6HH0M 3Ha^eHO pH (5-6) 30 uhh c 1,2 κγ ÓeHTOHHTa, OTca-cbiBaioT *iepe3 cjiofí sumflpaTa cepHOKHCjioro KaJiBHHH h $hjibt-paT BbiÓpacHBaioT. Cynnca cmoch BjiascHhifí Mmiejmfí—óohtohht nonpMMepy I saeT 2,8 κγ cTOfíKOfí npn xpaHOHMu cMecn cyxofíMHIieJIHfí-ύθΗΤΟΗΗΤ, KOTOpafl COflepOT aHaJMTHqeCKH Onpe£eJieH-'ΗΝΘ B KyJIBTypaJIBHOií CycnQH3HM aJIKaJIOMAhl (3ΡΓ03ΜΗ/ 3ΡΓ03Η-hhh/ cjiejm xaHOKjiaBHHa) npaKTHnecKH 100%. 3KCTpaKUHOHHuít 3φφβκτ npn aKCTpaKuo c nepeiíeinMBaHMeu cI0-I2-KpaTHmá KOjinqacTBOM sToaiíeiaia cocTaBJíaeT b cpea-Ηβω 90% b pacneTe Ha coflepxaHHe CMecu cyxofí uniiejiHfí-óeH-TOHHT. ΠρΗΜβρ 6 20 ji KyjiBTypajiBHořt cycneH3O ímaMMa, npuBejieHHoro b npn-uepe 5, φΗΒΒτργιοτ <5β3 soúaBJíeHHH ascopÓeHTa ηβρβ3 20 uu-Bufí cjiofí flurnapaTa cepHOKHCJioro κβτιβιιηη; φιυΐΒτρθτ, co-flepsamHií tojibko cjiejuj 3pro3HHa H qacTB conyTCTByiomHx aji-KajioooB, BhiópacbiBaDT. BuaejieHHHfí BJiaratifí MHuejiHfl cpaeyse cyinaT b ποθβαοοοκθηηομ cjioq πρκ 90 0 ao TeunepaTyptiOTxojiHmero B03ayxa 60 o(npoaojisMTejiBHOCTB okojio 40 mmh).IIojiynaiQT 0,8 ao 1,0 κγ CTOfíKoro npn χρβΗβΗΗΜ cyxoro uHiie-jihh, KOTopuft coaepxMT 96-100% onpejiejieHHoro b KyjiLTypaJiB-hoíí cycneH3HH 3pro3HHa, a laKse cjieflH conyTCTBywx ajiKaji-ΟΗΛΟΒ. TIjih nojiyneHHH aJiKajionsa cyxofí MHijejiHfí nocjie 3aueiiiHBaHHHc 150 ují 10%-HOfí aMMHa^HOfí bojuj 3KCTparHpyioT πρπ nepe-ueinHBaHHH c 8 ji xJIopoφopMa b AByx nopuHHx h nocjie πβρβΒΟ-Jia b BOíHO-KHCJiyio $a3y, pesKCTpaKiio h BunapHBaHHH H3nojiyneHHoro KOHueHTpaTa ocasflaioT BMHHOfí khcjiotoíí b βηλθTapTpaTa-cupiia· 6 Τ-
ΦΟΡΜΠΑ H30EPETEHHH Ι. Cnocotf ΒΗΑθΤΙΘΗΗΗ aJIKaJIOH^OB CnOpHHBH H3 KyjIBTyp3JIBHKXcycneH3Hií, oTJiH^aminHiícfl Ten, ητοcoópaHHyio KyjiLTypajiLHya cycneH3Hio b θοτθοτβθηηομ coc-TOHHHH nocne ΠθρθΜθΙΠΗΒΘΗΗΗ C ΓίΙΗΗ03ΘΜ01ί, CnOCOÓHHM KHatfyxaHMio, MexaHnqecKH pa3sejiaioT, HanpuMep, φρυικτρο-iíneft, CMecL BJiaratift MHnejiHíi-aflco*<3eHT cyrnaT b nceB^o-ΟΗΟθΗΗΟΜ caoe, CMeiDHBaioT fljifl HaÓyxaHHH c auiínaqHOfí bo-floft, 3KCTparnpyiQT opraHuneoKnun, anpoTOHHuuH pacTsopii-τβΗΗωΗ h sKCTpaKT nepepatfaTHBaioT H3BecTHhiM oópa3OM· 2. Cnocoó no nyHKTy I, OTíímaiomHftcfl τ e m ,ητο b KanecTBe rjiHH03eMa, cnocoÓHoro κ HaÚyxaHHio, npn-μθηηιοτ oi 4 jo 5 b6cobhx προίξβΗΤΟΒ ÓSHTOHHTa h napě#líexaHHnecKHM pa3AeJieHneu KyjiBTypaJiBHyro cycneH3HS) nepe-MeniHBaioT c aacopÓeHTOM b TeneHae 30 mhh. 3. Cnocoó no nyHKTy I, OTJinnaioinHíícH τ e m,hto cyuiKy cmsch BjiasHHií Munejinil-ascopÚeHT ocyíjecTBJíHioTB ΠΟβΒβΟΟΜΚΘΗΗΟΜ CJlOe ΠρΗ 80-90 °C B ΤβΗ6ΗΗ6 20-40 Λ’ΠΗΛΟ TeMnepaTypu oTxo^flinero B03syxa 50-70 °C w οοτθτοηηοΚBJiam He Óojiee 15 %· 4. Cnocotf no nyHKTy I, OTamaioinHcfl τ e m,hto b KanecTBe anpoTOHHhtx pacTBopuTeneit ajih sKCTpaKHOTBepAoe BemecTBO-oaKOCTB πρημθηηώτ ΗΗ3ΠΜ6 δφηρυ ajiKHji-KapÓOHOBOří khcjioth, npenuymecTBeHHO sToaneTaT , aneTOHhjih raJioreHHpoBaHHHe yrjieBOflopo/ní, npeHMymecTBeHHOΧίίοροφορω OH XJIOpHCTUÍÍ ΜβΤΟΘΗ, H Cld6CB CyXOÍÍ MHIjejIHÍÍ-a#copdeHT nepes sKCTpaKnnefí cweniHBaioT jjih HaOyxaHHH c10-20 Bec.% aMMiianHOií boali h sKCTpaKT-capen nepepaóa-TblBaiOT W3BeCTHblM 0Ópa30U. 7
<P l·
AHHOTAW C uíCCCOZ JTIT? 7;JI Jí H30ÓpSTQHHe OTHOCHTCH K OAHOpflSHOMy cnocody+BHAejieHHHajiKajiOHaoB cnopuHLH H3 KyjiLTypajiLHLix cycneH3Míí.
Oh npesHasHa^eH ajih npoMuuuieHHoro nojiy^eHMH amcaJiOHAOBcnoptíHBH a ji η TspaneBTH^acKHx ijejieft.
Uqjib M30ópeTehHH 3aKJUouaJiaci> b pa3paúOTKe yHHBepcaJimoΠρΜΜΘΗΜΜΟΓΟ ΟΑΗΟρΗΑΗΟΓΟ ClIOCOÓa ΙψΤθΜ ΠθρθΒΟΑβ COBOKyn-hocth ajiKaJioHjjOB b ycTOíiqHBbiří κ xpaHSHHK), 3KCTparnpHye-unii npenapaT cyxoro ΜΗΐξβπΜΗ.
CymKOCTB H30Óp6T6HHfl COCTOHT B aflCOpÓItfJH paCTBOpSHHOÍÍHacTH anKaJiowB ciiocoOhum κ HaúyxaHHio γαηηο36μομ, otac-JI6HHH $HJIBTpaTa H CyiHKe BJiaJKHOIO MHqejIHH HJIH cuecu BJia:?C-HNÍÍ MHUejIHÍi-aACOpÓeHT B ΠΟβΒΑΟΟΚΗΚβΗΗΟΜ CJIOe. IlOCJie 3K-CTpaKUHH cyxoro mhiíoamh hah cuecu eyxoft MHuejiHií-aAcopúaHTOpraHM^eCKHMH, H6CM6IflHBai01HHMHCfl C BOAOÍÍ paCTBOpiITeJIHMH,ajiKaJiOHAH πθρθβοαητ b bqaho—KHCJiyio $a3y h nocjie no#ne-jia^HBaHHH pesKCTpampyiOT. •BO3MOSHLIMH OÓJiaCTHMH ΠρΗΜΘΗβΗΗΗ Η300ρθΤβΗΗΗ M03CH0 Η33Β3ΤΒΒΗΑθπθΗΗΘ ΠΘΠΤΗΑΗΗΧ aAK3JI0HA0B Η/HJIH BOAOpaCTBOpHMhlXaJiKaJiOHAQB cnopHHLM M3 KyjiLTypauLHLix cycneH3Hfl, ocoóeHHOH3 rJiyOMHHhlX H B03SyiHHLIX KyJIBTyp CO CneKTpOM, BKJIIOqaiO-mHM HeCKOJIBKO aJIKaJIOHAOB pa3JIH<ffl0ft paCTBOpHMOCTH, 8

Claims (4)

  1. 9 PŘEDMĚT VYNÁLEZU
    1. Způsob isolace námelových alkaloidů z kultivační'sus-penze, vyznačující se tím,že sebraná kultivační sus-penze v přírodním stavu se smísí s kysličníkem hlini-tým,schopným botnání, mechanicky se oddělují napříkladfiltrací, směs .vlhké mycelium-adsorbent se suší v fluidní vrstvě, za účelem botnání se smíchává s čpavkovouvodou, extrahují se organickými aprotickými rozpou-štědly a extrakt se zpracovává známým způsobem.
  2. 2. Způsob podle bodu 1, vyznačující se tím, že jako kys-ličníku hlinitého, schopného botnání, používají od 4do 5 hmotn. % bentonitu a před mechanickým oddělenímkulturovou suspenzi se smíchá s adsorbentem po dobu30 minut.
  3. 3. Způsob podle bodu 1, vyznačující se tím, že sušení smě-si vlhký mycel-adsorbent uskutečňují v fluidizačnívrstvě při 50 až 90 °C po dobu 20 až 40 minut do tep-loty odcházejícího vzduchu 50 až 70 °C a do zbytkovévlhkosti méně než 15 %.
  4. 4. Způsob podle bodu 1, vyznačující se tím, že jako ap-rotická rozpouštědla pro extrakci pevná látka-kapali-na se použijí nižší estery alkylokarbonové kyseliny,převážně etylacetát, aceton nebo halogenované uhlo -vodíky, přednostně chloroform nebo metylénchlorid asměs suché mycelium-adsorbent před axtrakcí se smíchápo nabotnání s 10 až 20 hmotn. % čpavkové vody a ex-trakt-polotovar se zpracovává známým způsobem. Uznáno vynálezem na základě výsledků expertizy,prove-dené Úřadem pro vynálezectví a patentnictví, Berlín, DD
CS787736A 1977-12-20 1978-11-24 Method of izolating ergot alkaloids from cultivation suspensions CS217423B1 (en)

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DD20279877A DD138223B1 (de) 1977-12-20 1977-12-20 Verfahren zur isolierung von mutterkornalkaloiden aus kultursuspensionen

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JP (1) JPS559791A (cs)
AT (1) AT369784B (cs)
CH (1) CH638813A5 (cs)
CS (1) CS217423B1 (cs)
DD (1) DD138223B1 (cs)
DE (1) DE2840670A1 (cs)
FI (1) FI783930A (cs)
FR (1) FR2412546A1 (cs)
HU (1) HU179662B (cs)
SE (1) SE7813066L (cs)
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US5178832A (en) * 1987-09-28 1993-01-12 The Texas A&M University System Selective immobilization and detection of mycotoxins in solution
AU2722888A (en) * 1987-09-28 1989-04-18 The Texas A & M University System Selective immobilization and detection of mycotoxins in solution

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US2835675A (en) * 1951-11-02 1958-05-20 Abe Matazo Elymoclavine and manufacture of ergot alkaloids by culture
US2809920A (en) * 1953-04-10 1957-10-15 Saul & Co Process for the preparation of ergotamine, ergotaminine and ergometrine by saprophytic culture of ergot (claviceps purpurea [fr] tul.) in vitro and isolation of the alkaloids thus produced

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YU261878A (en) 1983-10-31
JPS559791A (en) 1980-01-23
DD138223A1 (de) 1979-10-17
HU179662B (en) 1982-11-29
DD138223B1 (de) 1980-12-24
FI783930A (fi) 1979-06-21
FR2412546A1 (fr) 1979-07-20
US4237291A (en) 1980-12-02
SU985020A1 (ru) 1982-12-30
CH638813A5 (de) 1983-10-14
AT369784B (de) 1983-01-25
SE7813066L (sv) 1979-06-21
FR2412546B1 (cs) 1983-07-22
DE2840670A1 (de) 1979-07-19

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