• 제목/요약/키워드: semipreparative HPLC

검색결과 10건 처리시간 0.024초

천연 latex로부터 ${\alpha}-,\;{\gamma}-,\;{\delta}-tocotrienol$의 분리 (Separation of ${\alpha}-,\;{\gamma}-,\;{\delta}-tocotrienol$ from latex)

  • 이형옥
    • Applied Biological Chemistry
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    • 제36권1호
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    • pp.29-32
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    • 1993
  • Latex(Hevea Brasiliensis)로부터 3종의 ${\alpha}-,\;{\gamma}-,\;{\delta}-tocotrienol$을 각각 분리하고, oil 상태의 각 성분을 얻었다. Tocotrienol을 분리하기 위하여, latex에서 추출한 조지방 성분의 비비누화분획으로 부터 semipreparative HPLC에 의한 분리방법을 사용하여 tocotrienol을 분리하였다. 이와 같은 분리방법을 이용하였을 때 latex에 함유된 tocotrienol의 함량은 약 400ppm이었으며, 순도는 ${\alpha}-,\;{\gamma}-,\;{\delta}-tocotrienol$ 각각 98.3, 99.3, 96.2%로 나타났다.

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개 혈소판에서 변형성장인자 베타의 분리에 관한 연구 (Study on the Purification of Transforming Growth Factor-$\beta$ in Canine Platelets)

  • 권오경;홍성혁
    • 한국임상수의학회지
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    • 제11권1호
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    • pp.389-392
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    • 1994
  • To purify transforming growth factor type beta(TGF-$\beta$) in canine platelets, Sephadex G-75 gel filtration and semipreparative HPLC were carried out. The column of $2.0 {\times}120cm$ was used for gel filtration and one inch semipreparative column filled with SP-Toyopeal for HPLC. Electrophoresis and bioassay using African green monkey kidney cell were used for identification of TGF-$\beta$ Crude TGF-$\beta$ of 2.75mg was extracted from 5.2g of the platelets by the treatment of acid/ethanol. In gel filtration of crude TGF-$\beta$, 4 peaks were observed at the detection of spectrophotometer at 280nm. Electrophoresis and bioassay identified the 3rd peak TGF-$\beta$. Linear gradient elution from 0 to 3M NaCl in sornipreparative HPLC showed TGF-$\beta$ at 1.5M NaCl. Gel filtration was less expensive and useful method for the purification of TGF-$\beta$.

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시판 기능성식품으로부터의 실데나필 유도체 부정첨가물질의 분리 및 구조규명 (Isolation and Identification of an Unauthorized Sildenafil Analogue in a Commercial Functional Food)

  • 백두종
    • 대한화학회지
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    • 제54권4호
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    • pp.443-446
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    • 2010
  • 기능성식품으로 시판되는 건강음료를 HPLC 분석한 결과 발기부전치료제로 허가받은 비아그라$^{(R)}$의 활성주성분인 실데나필과 구조적으로 유사한 부정첨가물질이 발견되었다. 이 부정첨가물질의 구조를 규명하기 위해 건강음료를 methylene chloride로 추출한 다음 그 추출물을 semipreparative HPLC로 정제하였다. 분리된 물질의 화학구조는 IR, LC/MS-ESI, NMR 분광학으로 규명하였는데 실데나필과 유사한 특징을 보였고 구조상의 유일한 차이는 실데나필의 methylpiperazine 부분구조를 부정첨가물질에서 hydroxyethylpiperazine으로 치환한 것이었다.

시판 기능성식품으로부터의 타다라필 유도체 부정첨가물질의 분리 및 구조규명 (Isolation and Identification of an Unauthorized Tadalafil Analogue in a Commercial Functional Food)

  • 백두종
    • 약학회지
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    • 제54권4호
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    • pp.240-243
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    • 2010
  • High-performance liquid chromatography (HPLC) screening method revealed that a propolis product marketed as a functional food contained an undeclared substance similar to tadalafil, the active ingredient of the prescription drug Cialis$^{(R)}$ approved for the treatment of male erectile dysfunction. In order to identify the illegal additive, the propolis product was extracted with methylene chloride, and the extract was purified further using semipreparative HPLC. The chemical structure of the isolated substance was elucidated based on IR, LC/MS-ESI, and $^1H$- and $^{13}C$-NMR spectroscopy, which showed the characteristics similar to tadalafil. The only difference was the substitution of the methyl group at the piperazinedione ring of tadalafil to the amino group of the identified illegal additive.

Structural Analysis of Black Common Bean (Phaseolus vulgaris L.) Anthocyanins

  • Choung, Myoung-Gun
    • Food Science and Biotechnology
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    • 제14권5호
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    • pp.672-675
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    • 2005
  • Two anthocyanins were isolated from 1% HCl-20% methanol extracts of KG 97287 black common bean (Phaseolus vulgaris L.) using semipreparative, high-performance liquid chromatography (HPLC). The anthocyanins were identified using a combination of LC/ES-mass spectrometry (MS) and spectroscopic methods of UV-Vis, $^1H-$ and $^{13}C-$ nuclear magnetic resonance (NMR). The chemical structures of these two anthocyanins were elucidated as delphinidin 3-glucoside and petunidin 3-glucoside and their contents in KG 97287 black common bean seed coats were determined to be $2.614{\pm}0.11$ and $0.167{\pm}0.01\;mg/g$, respectively. These contents were lower than reported internationally and we recommend the introduction into Korea of high anthocyanin varieties of black common bean.

고속액체(高速液體) chromatography에 의(依)한 Ginsenoside $-Rb_1,\;-Rb_2,\;-Rc,\;-Rd,\;-Re$$-Rg_1$의 대량분리(大量分離) (Larqe guantity isolation of Ginsenoside $-Rb_1,\;-Rb_2,\;-Rc,\;-Rd,\;-Re\;and\;-Rg_1$ in Panax ginseng C.A. Meyer by High Performance Liquid Chromatography)

  • 최진호;김우정;배효원;오성기;대포언길
    • Applied Biological Chemistry
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    • 제23권4호
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    • pp.199-205
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    • 1980
  • 인삼의 유효약리성분으로 밝혀진 saponin중의 각 ginsenosides를 효과적이고 능률적으로 분리하기 위하여 대량분취전용 고속액체 chromatograph인 preparative HPLC의 응용을 검토하였다. 조(粗) saponin획분을 preparative HPLC인 Prep LC/system-500를 사용하여 부분분획을 하고 각 획분에 함유되어 있는 ginsenosides의 조성을 Analytical HPLC로 동정한 후 Semi-preparative HPLC를 사용하여 인삼주성분 saponin을 단리했다. 그 결과 인삼 주성분 saponin인 $ginsenoside-Rb_1,\;-Rb_2,\;-Rc,\;-Rd,\;-Re$$-Rg_1$은 약 20 mg / 2.0 ml / injection으로 chromatography를 행하여 $300{\sim}400mg/day$로 대량분취가 가능하였다. 따라서 ginsenosides의 약리 및 임상효능 연구에 크게 기여하게 될 것이다.

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Isolation of ginsenosides Rb1, Rb2, Rc Rd, Re, Rf and Rg1 from cinseng root by high performance liquid chromatography

  • Paik, Nam-Ho;Park, Man-Ki;Choi, Kang-Ju;Cho, Yung-Hyun
    • Archives of Pharmacal Research
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    • 제5권1호
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    • pp.7-12
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    • 1982
  • Ginsenosides Rb1, Rb2, Rc, Rd, Re, Rf and Rg1 were effectively isolated from ginseng root by preparative liquid chromatography (LC) on two PrepPAK-500/c18 cartridges in series and semipreparative LC on a .mu. Bondapak cabohydrate analysis column, a .mu.Bondapak C18 column or a .mu. Porasil column. The identities of the isolated ginsenosides were confirmed by analytical high-performance liquid chromatography (HPLC) and infrared spectrophotometry. By this method large scale isolation of pure ginsenosides was efficiently accomplished.

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고속액체(高速液體) 크로마토그래피에 의(依)한 Ginsenoside ${-Rh}_1$${-Rh}_2$ 의 분리(分離) (Isolation of Ginsenoside${-Rh}_1$ and ${-Rh}_2$ by High Performance Liquid Chromatography)

  • 최진호;김우정;홍순근;오성기;대포언길
    • 한국식품과학회지
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    • 제13권1호
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    • pp.57-66
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    • 1981
  • 인삼주성분 사포닌 및 미량성분 사포닌의 단리법에 대하여 HPLC의 응용을 검토하여 이미 보고한 바 있다. 따라서 인삼미량성분인 $Ginsenoside-Rh_1$ 및 미지성분인 $Ginsenoside-Rh_2$의 단리법을 검토하였다. 저자등의 방법에 따라 홍삼의 70% 에탄올추출액(4 kg)에서 부탄올추출액을 얻어 에틸 아세테이트로 처리 (실온에서 3시간 및 $60^{\circ}C$에서 3 시간)하여 에틸 아세테이트 획분(29g)을 preparative HPLC인 prep LC/System-500을 사용하여 부분분획하여 각 획분을 analtical HPLC/ALC-201로 동정, ginsenoside-Rh group을 다시 에테르, 에틸 아세테이트 및 물로 정제한 후, semipreparative HPLC/ALC-201로 $ginsenoside-Rh_1$$-Rh_2$를 단리했다. 미지성분단리에 HPLC의 응용이 효과적임이 판명되었다.

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Bioactivity-guided isolation of ginsenosides from Korean Red Ginseng with cytotoxic activity against human lung adenocarcinoma cells

  • Yu, Jae Sik;Roh, Hyun-Soo;Baek, Kwan-Hyuck;Lee, Seul;Kim, Sil;So, Hae Min;Moon, Eunjung;Pang, Changhyun;Jang, Tae Su;Kim, Ki Hyun
    • Journal of Ginseng Research
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    • 제42권4호
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    • pp.562-570
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    • 2018
  • Background: Lung cancer is the leading cause of cancer-related death worldwide. In this study, we used a bioactivity-guided isolation technique to identify constituents of Korean Red Ginseng (KRG) with antiproliferative activity against human lung adenocarcinoma cells. Methods: Bioactivity-guided fractionation and preparative/semipreparative HPLC purification were used with LC/MS analysis to separate the bioactive constituents. Cell viability and apoptosis in human lung cancer cell lines (A549, H1264, H1299, and Calu-6) after treatment with KRG extract fractions and constituents thereof were assessed using the water-soluble tetrazolium salt (WST-1) assay and terminal deoxyribonucleotidyl transferase-mediated dUTP nick end labeling (TUNEL) staining, respectively. Caspase activation was assessed by detecting its surrogate marker, cleaved poly adenosine diphosphate (ADP-ribose) polymerase, using an immunoblot assay. The expression and subcellular localization of apoptosis-inducing factor were assessed using immunoblotting and immunofluorescence, respectively. Results and conclusion: Bioactivity-guided fractionation of the KRG extract revealed that its ethyl acetate-soluble fraction exerts significant cytotoxic activity against all human lung cancer cell lines tested by inducing apoptosis. Chemical investigation of the ethyl acetatesoluble fraction led to the isolation of six ginsenosides, including ginsenoside Rb1 (1), ginsenoside Rb2 (2), ginsenoside Rc (3), ginsenoside Rd (4), ginsenoside Rg1 (5), and ginsenoside Rg3 (6). Among the isolated ginsenosides, ginsenoside Rg3 exhibited the most cytotoxic activity against all human lung cancer cell lines examined, with $IC_{50}$ values ranging from $161.1{\mu}M$ to $264.6{\mu}M$. The cytotoxicity of ginsenoside Rg3 was found to be mediated by induction of apoptosis in a caspase-independent manner. These findings provide experimental evidence for a novel biological activity of ginsenoside Rg3 against human lung cancer cells.

맥문동 종실 안토시아닌 분획물의 멜라닌 생성 억제 및 미백 효과 (Antimelanogenic Effect and Whitening of Anthocyanin Rich Fraction from Seeds of Liriope platyphylla)

  • 정명근;황영선;김기쁨;안경근;심훈섭;홍승범;최재후;유창연;정일민;김승현;임정대
    • 한국약용작물학회지
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    • 제21권5호
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    • pp.361-371
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    • 2013
  • This study was performed to determine the antimelanogenic effect and tyrosinase inhibitory activities of anthocyanin rich fraction (AN-SLP) from Liriope platyphylla Wang et Tang seeds. Anthocyanins isolated from L. platyphylla seeds revealed the presence of four major anthocyanin components, which were tentatively identified as delphinidin-3-Oglucoside, delphinidin-3-O-rutinoside, petunidin-3-O-rutinoside, and malvidin-3-O-rutinoside using semipreparative HPLC, $^1H$-NMR, $^{13}C$ NMR, FAB-MS and LC/ES-MS. The inhibitory effect of AN-SLP on tyrosinase activity was studied using in vitro (against mushroom tyrosinase) and ex vivo (against B16 melanoma cell tyrosinase) models. Cellular tyrosinase activity was decreased by AN-SLP treatment in B 16 melanoma cells through dose dependent manner, but AN-SLP did not inhibit mushroom tyrosinase and L-DOPA oxidation directly. AN-SLP showed melanin inhibition by 53.2% at 50 ${\mu}g/m{\ell}$ which was 0.7 times more efficient than the antimelanogenic effect of commercial arbutin and kojic acid (36.5%) also did not show cell toxicity. Additionally, AN-SLP inhibited the activity of ${\alpha}$-glucosidase and the glycosylation of tyrosinase in melanoma cell. The resulting unsaturated glycosylation of tyrosinase makes it unstable and disturb correct transportation. From theses results, we conclude that AN-SLP could be used as anti-melanogenic agent for skin whitening.