CS217423B1 - Method of izolating ergot alkaloids from cultivation suspensions - Google Patents
Method of izolating ergot alkaloids from cultivation suspensions Download PDFInfo
- 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
- Authority
- CS
- Czechoslovakia
- Prior art keywords
- adsorbent
- mixed
- swelling
- process according
- iso iso
- Prior art date
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Classifications
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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
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- 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
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- 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)
- 9 PŘEDMĚT VYNÁLEZU1. 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. 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. 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. 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
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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DD20279877A DD138223B1 (de) | 1977-12-20 | 1977-12-20 | Verfahren zur isolierung von mutterkornalkaloiden aus kultursuspensionen |
Publications (1)
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CS217423B1 true CS217423B1 (en) | 1983-01-28 |
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CS787736A CS217423B1 (en) | 1977-12-20 | 1978-11-24 | Method of izolating ergot alkaloids from cultivation suspensions |
Country Status (13)
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US (1) | US4237291A (cs) |
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) |
SU (1) | SU985020A1 (cs) |
YU (1) | YU261878A (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 |
Family Cites Families (2)
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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 |
-
1977
- 1977-12-20 DD DD20279877A patent/DD138223B1/de unknown
-
1978
- 1978-09-19 DE DE19782840670 patent/DE2840670A1/de not_active Withdrawn
- 1978-09-25 AT AT0690378A patent/AT369784B/de not_active IP Right Cessation
- 1978-11-02 JP JP13566478A patent/JPS559791A/ja active Pending
- 1978-11-10 YU YU02618/78A patent/YU261878A/xx unknown
- 1978-11-22 SU SU787770363A patent/SU985020A1/ru active
- 1978-11-24 CS CS787736A patent/CS217423B1/cs unknown
- 1978-12-06 HU HU78AE554A patent/HU179662B/hu unknown
- 1978-12-19 SE SE7813066A patent/SE7813066L/xx unknown
- 1978-12-20 CH CH1295778A patent/CH638813A5/de not_active IP Right Cessation
- 1978-12-20 FI FI783930A patent/FI783930A/fi unknown
- 1978-12-20 US US05/971,219 patent/US4237291A/en not_active Expired - Lifetime
- 1978-12-20 FR FR7835845A patent/FR2412546A1/fr active Granted
Also Published As
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ATA690378A (de) | 1982-06-15 |
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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SU422161A3 (ru) | СПОСОБ ПОЛУЧЕНИЯ СЛОЖНЫХ ЭФИРОВ СУЛЬФОКСИДА 7-АЦИЛАМИНО-З-АЦИЛОКСИМЕТИЛ-ДЗ-ЦЕФАЛОСПОРИНА1Изобретение относитс к улучшенному способу получени производных цефалоспорина, которые могут найти применение в фармацевтической промышленности.Известен способ получени сульфоксида 7- ациламино-А^(или А^)-цефалоспоринов общей формулыСО ОБ.где R — ацильна группа;X — водород или нуклеофильна группа;R' — водород, силильна группа или алкил или аралкил с 1—20 атомами углерода, заключающийс в том, что соответствующий 7- ациламидо-А^(или А^)-цефалоспорин подвергают окислению надкислотой или перекисью водорода в присутствии кислоты, с последующим выделением продуктов известным способом.Согласно предлагаемому изобретению дл упрощени процесса предложено проводить функционализацию экзоциклической оксиме- тильной группы в положении 3 сульфоксида10157-ациламинодезаметилцефалоспорина без попутной изомеризации двойной св зи цефало- споранового кольца при получении известных антибиотиков типа цефалоспорина.Описываемый способ получени эфиров сульфоксида 7-ациламино-3-оксиметил-А2-це- фалоспоринов общей формулыОкосш,^it"^Y^CH^OCOR, СООБ.12025где R — ацильный остаток;RI — остаток защитной группы, включающей С4—Сб-трет-алкил, Cs—Ст-грет-алкенил, Сз—• Сг-ГуОет-алкинил, бензил, метоксибензил, нит- робензил, фенацил, трихлорэтил, бензгидрил, фталимидометил, метилимид нтарной кислоты;R2-^ остаток ангидрида алифатической кар- боновой кислоты, содержащего от 4 до 20 атомов углерода,заключаетс в том, что сульфоксид 7-ацил- аминодезацетилцефалоспорина общей формулы |