KR970701786A - 스트렙토마이세스 sp. P 6621 FERM P 2804의 발효액으로부터 클라불란산과 제약학적으로 허용가능한 이들의 염을 단리하는 신규한 방법(NOVEL PROCESS FOR THE ISOLATION OF CLAVULANIC ACID AND OF PHARMACEUTICALLY ACCEPTABLE SALTS THEREOF FROM THE FERMENTATION BROTH OF STREPTOMYCES SP. P 6621 FERM P 2804) - Google Patents
스트렙토마이세스 sp. P 6621 FERM P 2804의 발효액으로부터 클라불란산과 제약학적으로 허용가능한 이들의 염을 단리하는 신규한 방법(NOVEL PROCESS FOR THE ISOLATION OF CLAVULANIC ACID AND OF PHARMACEUTICALLY ACCEPTABLE SALTS THEREOF FROM THE FERMENTATION BROTH OF STREPTOMYCES SP. P 6621 FERM P 2804)Info
- Publication number
- KR970701786A KR970701786A KR1019960704806A KR19960704806A KR970701786A KR 970701786 A KR970701786 A KR 970701786A KR 1019960704806 A KR1019960704806 A KR 1019960704806A KR 19960704806 A KR19960704806 A KR 19960704806A KR 970701786 A KR970701786 A KR 970701786A
- Authority
- KR
- South Korea
- Prior art keywords
- streptomyces
- fermentation broth
- clavulanic acid
- pharmaceutically acceptable
- ferm
- Prior art date
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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
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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
- C12P17/188—Heterocyclic compound containing in the condensed system at least one hetero ring having nitrogen atoms and oxygen atoms as the only ring heteroatoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D503/00—Heterocyclic compounds containing 4-oxa-1-azabicyclo [3.2.0] heptane ring systems, i.e. compounds containing a ring system of the formula:, e.g. oxapenicillins, clavulanic acid derivatives; Such ring systems being further condensed, e.g. 2,3-condensed with an oxygen-, nitrogen- or sulfur-containing hetero ring
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- C12N1/00—Microorganisms, e.g. protozoa; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor
- C12N1/02—Separating microorganisms from their culture media
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S435/00—Chemistry: molecular biology and microbiology
- Y10S435/8215—Microorganisms
- Y10S435/822—Microorganisms using bacteria or actinomycetales
- Y10S435/886—Streptomyces
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Zoology (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Biotechnology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Genetics & Genomics (AREA)
- General Health & Medical Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Microbiology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Biomedical Technology (AREA)
- Virology (AREA)
- Tropical Medicine & Parasitology (AREA)
- Medicinal Chemistry (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Micro-Organisms Or Cultivation Processes Thereof (AREA)
- Nitrogen And Oxygen Or Sulfur-Condensed Heterocyclic Ring Systems (AREA)
- Seasonings (AREA)
Abstract
본 발명은 발효액으로부터 대부분의 균사, 단백질 및 다른 부유하는 고체 입자들을 약 20 내지 40℃ 사이에서 pH가 5.8 내지 6.2인 배지에서 미세 여과에 의해 제거하고, 정제된 액(수성층)을 임의로 한외 여과법에 의해 재차 정체한 후 이 정제된 액을 역삼투에 의해 농축하고, 이어서 pH가 1 내지 3인 배지에서 물에 섞이지 않은 유기 용매로 원심분리 추출기 내에서 역류로 직접 추출하여 여전히 남아있는 단백질을 동시에 제거하고, 얻어진 유기층으로부터 유기층을 물로 세척함으로써 수용성 불순물을 제거하고, 상기 유기층은 정유관에서 진공하에서 0.1부피% 이하의 수분 함량으로 건조하고, 증발에 의해 농축하고, 활성탄으로 처리하여 탈색한 후 건조된 유기층에 존재하는 클라불란산을 가장 적당하게 에틸 아세테이트상에서 단리하고 실온 정도에서 N,N'-디이소프로필에틸렌디아민과 반응시켜 중간 단계의 N,N'-디이소프로필에틸렌디암모늄 디클라불라네이트로 정제하고, 이것을 단리하여 칼륨 2-에틸 헥사노에이트의 이소프로판을 용액과 반응시켜 고순도의 클라불란산 칼륨염을 얻는 것을 특징으로 하느 스트렙토마이세스 sp. P 6621 FERM P 2804의 수성 발효액으로부터 클라불란산과 제약학적으로 허용가능한 이들의 염을 단리하는 방법에 관한 신규하고 개선된 방법에 관한 것이다.
Description
본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음
Claims (5)
- 발효액으로부터 대부분의 균사, 단백질 및 다른 부유하는 고체 입자들을 약 20 내지 40℃ 사이에서 pH가 5.8 내지 6.2인 배지에서 미세 여과에 의해 제거하고, 정제된 액(수성층)을 임의로 한외 여과법에 의해 재차 정제한 후, 이 정제된 액을 역삼투에 의해 농축하고, 이어서 pH가 1 내지 3인 배지에서 물에 섞이지 않는 유기 용매로 일련의 원심분리 추출기로 역류로 직접 추출하여 여전히 남아있는 분리된 단백질을 동시에 제거하고, 유기층을 물로 세척하고, 정유관에서 진공 하에서 0.1부피% 이하의 수분 함량으로 건조하고, 증발에 의해 농축하고, 활성탄으로 처리하여 탈색한 후 완전히 건조된 유기층에 존재하는 클라불란산을 단리하고 실온 정도에서 N,N'-디이소프로필에틸렌디아민과 반응시켜 N,N'-디이소프로필에틸렌디암모늄 디클라불라네이트로 정제하고, 이것을 단리하여 칼륨 2-에틸 헥사노에이트의 이소프로판을 용액과 반응시켜 고순도의 클라불란산 칼륨염을 얻는 것을 특징으로 하는 스트렙토마이세스 sp. P 6621 FERM P 2804의 수성 발효액으로부터 클라불란산과 제약학적으로 허용가능한 이들의 염을 단리하는 방법.
- 제1항에 있어서, 배지의 pH가 황산으로 조절되는 것을 특징으로 하는 스트렙토마이세스 sp. P 6621 FERM P 2804의 수성 발효액으로부터 클라불란산과 제약학적으로 허용가능한 이들의 염을 단리하는 방법.
- 제1항에 있어서, 직접 추출시 물에 섞이지 않는 유기 용매로 에틸아세테이트가 사용되는 것을 특징으로 하는 스트렙토마이세스 sp. P 6621 FERM P 2804의 수성 발효액으로부터 클라불란산과 제약학적으로 허용가능한 이들의 염을 단리하는 방법.
- 제1항에 있어서, 정제된 수성 발효액의 직접 역류추출이 15 내지 25℃ 사이에서 에틸 아세테이트로 실시되는 것을 특징으로 하는 스트렙토마이세스 sp. P 6621 FERM P 2804의 수성 발효액으로부터 클라불란산과 제약학적으로 허용가능한 이들의 염을 단리하는 방법.
- 제1항에 있어서, 유기층의 건조에서 수분 함량이 0.03 내지 0.05부피%인 것을 특징으로 하는 스트렙토마이세스 sp. P 6621 FERM P 2804의 수성 발효액으로부터 클라불란산과 제약학적으로 허용가능한 이들의 염을 단리하는 방법.※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SIP-9400107 | 1994-03-02 | ||
SI9400107A SI9400107A (en) | 1994-03-02 | 1994-03-02 | New process of the isolation of clavulanic acid and its pharmaceutical salts from fermented broth of streptomyces sp.p 6621 ferm p 2804. |
PCT/SI1995/000002 WO1995023870A1 (en) | 1994-03-02 | 1995-02-23 | Novel process for the isolation of clavulanic acid and of pharmaceutically acceptable salts thereof from the fermentation broth of streptomyces sp. p 6621 ferm p 2804 |
Publications (2)
Publication Number | Publication Date |
---|---|
KR970701786A true KR970701786A (ko) | 1997-04-12 |
KR100293172B1 KR100293172B1 (ko) | 2001-06-15 |
Family
ID=20431337
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
KR1019960704806A KR100293172B1 (ko) | 1994-03-02 | 1995-02-23 | 스트렙토마이세스sp. P6621 FERM P2804의 발효액으로부터 클라불란산과 제약학적으로 허용가능한 이들의 염을 단리하는 신규한 방법 |
Country Status (25)
Country | Link |
---|---|
US (4) | US5780274A (ko) |
EP (1) | EP0748387B1 (ko) |
JP (1) | JP2948661B2 (ko) |
KR (1) | KR100293172B1 (ko) |
CN (1) | CN1055694C (ko) |
AT (1) | ATE159549T1 (ko) |
AU (1) | AU694176B2 (ko) |
BG (1) | BG62213B1 (ko) |
CA (1) | CA2184619A1 (ko) |
CZ (1) | CZ284117B6 (ko) |
DE (1) | DE69500925T2 (ko) |
DK (1) | DK0748387T3 (ko) |
ES (1) | ES2108572T3 (ko) |
FI (1) | FI963408A (ko) |
GR (1) | GR3025942T3 (ko) |
HU (1) | HUT74944A (ko) |
NO (1) | NO318374B1 (ko) |
NZ (1) | NZ279958A (ko) |
PL (1) | PL180520B1 (ko) |
RO (1) | RO118760B1 (ko) |
RU (1) | RU2206613C2 (ko) |
SI (1) | SI9400107A (ko) |
SK (1) | SK279780B6 (ko) |
WO (1) | WO1995023870A1 (ko) |
ZA (1) | ZA951689B (ko) |
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SI9400107A (en) * | 1994-03-02 | 1995-10-31 | Lek Tovarna Farmacevtskih | New process of the isolation of clavulanic acid and its pharmaceutical salts from fermented broth of streptomyces sp.p 6621 ferm p 2804. |
GB9500977D0 (en) * | 1995-01-19 | 1995-03-08 | Smithkline Beecham Plc | Novel process |
SI9500074A (en) † | 1995-03-10 | 1996-10-31 | Lek Tovarna Farmacevtskih | Process for preparation of alkani salts of clavulanic acid. |
SI9500134B (sl) | 1995-04-20 | 2004-04-30 | Lek, | Postopek za pripravo čistih alkalijskih soli klavulanske kisline |
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ATE273982T1 (de) | 2000-05-13 | 2004-09-15 | Smithkline Beecham Plc | Verfahren zur reinigung eines salzes der clavulansäure |
GB0022841D0 (en) * | 2000-09-18 | 2000-11-01 | Smithkline Beecham Plc | Process |
KR100443082B1 (ko) * | 2002-10-18 | 2004-08-04 | 삼성전자주식회사 | 반도체 장치의 트랜지스터 제조 방법 |
KR100768476B1 (ko) | 2005-11-24 | 2007-10-18 | 한국해양연구원 | 항암물질을 생산하는 방선균 스트렙토마이세스 속 균주,이의 분리방법, 이로부터 반고형 추출물을 제조하는 방법,이로부터 유래한 반고형 추출물 및 이를 이용한 항암제조성물 |
CN102838624B (zh) * | 2012-09-07 | 2014-10-29 | 安徽普朗膜技术有限公司 | 一种从发酵液中纯化克拉维酸的方法 |
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1994
- 1994-03-02 SI SI9400107A patent/SI9400107A/sl not_active IP Right Cessation
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1995
- 1995-02-23 DE DE69500925T patent/DE69500925T2/de not_active Expired - Fee Related
- 1995-02-23 RO RO96-01735A patent/RO118760B1/ro unknown
- 1995-02-23 ES ES95909194T patent/ES2108572T3/es not_active Expired - Lifetime
- 1995-02-23 DK DK95909194.3T patent/DK0748387T3/da active
- 1995-02-23 NZ NZ279958A patent/NZ279958A/en unknown
- 1995-02-23 EP EP95909194A patent/EP0748387B1/en not_active Expired - Lifetime
- 1995-02-23 CN CN95191927A patent/CN1055694C/zh not_active Expired - Fee Related
- 1995-02-23 WO PCT/SI1995/000002 patent/WO1995023870A1/en active IP Right Grant
- 1995-02-23 US US08/632,402 patent/US5780274A/en not_active Expired - Fee Related
- 1995-02-23 AT AT95909194T patent/ATE159549T1/de not_active IP Right Cessation
- 1995-02-23 CZ CZ962557A patent/CZ284117B6/cs not_active IP Right Cessation
- 1995-02-23 AU AU17241/95A patent/AU694176B2/en not_active Ceased
- 1995-02-23 RU RU96121357/13A patent/RU2206613C2/ru not_active IP Right Cessation
- 1995-02-23 JP JP7522554A patent/JP2948661B2/ja not_active Expired - Fee Related
- 1995-02-23 CA CA002184619A patent/CA2184619A1/en not_active Abandoned
- 1995-02-23 SK SK1120-96A patent/SK279780B6/sk unknown
- 1995-02-23 PL PL95316085A patent/PL180520B1/pl not_active IP Right Cessation
- 1995-02-23 KR KR1019960704806A patent/KR100293172B1/ko not_active IP Right Cessation
- 1995-02-23 HU HU9602351A patent/HUT74944A/hu unknown
- 1995-03-01 ZA ZA951689A patent/ZA951689B/xx unknown
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1996
- 1996-08-30 NO NO19963628A patent/NO318374B1/no unknown
- 1996-09-02 FI FI963408A patent/FI963408A/fi not_active IP Right Cessation
- 1996-09-02 BG BG100816A patent/BG62213B1/bg unknown
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1998
- 1998-01-16 GR GR980400112T patent/GR3025942T3/el unknown
- 1998-07-10 US US09/113,790 patent/US5985625A/en not_active Expired - Fee Related
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1999
- 1999-10-08 US US09/415,483 patent/US6207428B1/en not_active Expired - Fee Related
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