• 제목/요약/키워드: Chromatographic analyses

검색결과 61건 처리시간 0.025초

방선균 분리주가 생산하는 Phospholipase C 저해물질인 MT-2617-2B의 분리 및 특성 (Isolation and Characterization of MT2617-2B, a Phospholipase C Inhibitor Produced by an Actinomycetes Isolate)

  • 고학룡;이현선;오원근;안순철;김보연;강대욱;민태익;안종석
    • 한국미생물·생명공학회지
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    • 제24권1호
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    • pp.19-26
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    • 1996
  • A phospholipase C (PLC) inhibitor (MT267-2B) was isolated from the culture broth of actinomycetes isolate MT2617-2 by the extraction with n-butanol and column chromatographic techniques. The molecular weight of the inhibitor was 1057, by the spectroscopic analyses of IR, $^{13}C$-and $^{1}H$-NMR and ESI-MS. The chemical structure of MT2617-2B was found to be a macrolide compound consisted of a hemiketal ring, polyhydroxyl and polymethyl groups, which had a malonate and guanidine group as its side chain. MT2617-2B produced its two isomers having the same molecular weight by standing in methanol solution at room temperature. Therefore, MT2617-2B was identified as copiamycin and niphithricin A, macrolide antibiotics. The values of $IC_{50}$ against PLC-${\gamma}$1 and PLC-${\beta}$1 were 25 and 50${\mu}$g/ml, respectively. MT2617-2B had antimicrobial activities against Staphylococcus aureus and Candida albicans, but not against Escherichia coli.

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RP-HPLC-PAD를 이용한 갈근(葛根)과 갈근(葛根) 함유 처방의 Puerarin과 Daidzin 분석 (Determination Method of Puerarin and Daidzin from Puerariae Radix by Reversed-Phase HPLC with Pulsed Amperometric Detection)

  • 초진영;권하정;정지선;이제현;홍선표
    • 대한본초학회지
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    • 제23권4호
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    • pp.171-177
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    • 2008
  • Objectives: This study presents a reversed-phase high-performance liquid chromatography- pulsed amperometric detection(RP-HPLC-PAD) method for the determination of puerarin and daidzin in Puerariae Radix extract and Chinese medicinal preparations. Methods: Chromatographic separation was performed using a 10% acetonitrile with a reversed-phase column(Unison UK-C18, $100mm{\times}2.0mm$ I.D.; $3{\mu}m$). The analyses were detected by pulsed amperometric detector(PAD) in alkaline conditions by combining with post-column NaOH solution. Geniposide was used as an internal standard. Results: The limit of detection(S/N=3) and the limit of quantification(S/N=10) were 0.025 ng, 0.075 ng for puerarin, and 0.05 ng, 0.15 ng for daidzin, respectively. The intra- and inter-day precisions(RSDs) were less than 6.5% and average recoveries of puerarin were 99.7-101.3% and those of daidzin were 101.0-102.8%. Conclusions: According to above results, we developed a determination method for puerarin and daidzin in Puerariae Radix with high sensitivity and selectivitely.

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PVP 분리 수지에서 온도에 따른 당과 유기산의 체류 특성 변화 (Temperature Effect on the Retention Behavior of Sugars and Organic Acids on poly (4-vinylpyridine) Resin)

  • 김진일;이종호;구윤모
    • Korean Chemical Engineering Research
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    • 제44권1호
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    • pp.35-39
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    • 2006
  • 본 실험에서는 모델 시스템으로써 PVP 수지에서 과당, 포도당과 같은 당 시료와 젖산, 아세트산과 같은 유기산을 사용하여 온도 변화에 따른 체류 시간의 변화 정도를 알아보았다. 펄스 시험을 사용하여 당 시료의 온도 변화에 따른 체류 시간 변화를 알아본 결과, 그 변화가 크지 않았다. PVP 수지는 일반적으로 당 분리에 사용되는 분리 수지가 아닌 사실에서 예측할 수 있듯이 현저히 떨어지는 분리능을 보였고, 온도 변화에 따른 분리능의 변화 또한 나타나지 않았다. 반면에, PVP 수지에서 유기산의 경우에는 상당한 변화를 보였다. 따라서, 유기산에 대한 정량적 흡착특성의 변화를 알아보기 위하여 $35^{\circ}C$, $65^{\circ}C$ 온도에서 전단 분석하여 그 차이를 확인하였다. 이러한 온도에 대한 흡착특성은 SMB(simulated moving bed)와 같은 대규모 크로마토그래피 공정에 이용될 수 있을 것으로 판단한다.

Identification of Psychrophile Shewanella sp. KMG427 as an Eicosapentaenoic Acid Producer

  • Lee, Won-Hae;Cho, Ki-Woong;Park, Soo-Young;Shin, Kee-Sun;Lee, Dong-Sun;Hwang, Seon-Kap;Seo, Seok-Jong;Kim, Jong-Myeong;Ghim, Sa-Youl;Song, Bang-Ho;Lee, Sang-Han;Kim, Jong-Guk
    • Journal of Microbiology and Biotechnology
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    • 제18권12호
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    • pp.1869-1873
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    • 2008
  • An isolate from holothurians was identified as an eicosapentaenoic acid (EPA)-producing bacterium KMG427, which is characterized by EPA synthesis efficiency, by thin layer and gas chromatographic analyses. The EPA production was maximized to more than 10% of the total fatty acids by incubation at $4^{\circ}C$ after cell proliferation at $20^{\circ}C$. The isolated bacterium was categorized as Gram-negative, rod-shaped, aerobic, and motile with a single polar flagellum. According to phylogenetic analysis based on morphological and physiological specificities as an EPA-producing bacterium, the isolate KMG427 was found to belong to the genus Shewanella. The 16S rDNA of KMG427 was revealed to have 100% of sequence identity to that of S. hanedai CIP $103207^T$. Therefore, the isolate might be classified and identified as Shewanella sp. KMG427.

국산(國産) 마아가린중의 트란스산(酸) 함량 (Content of trans Fatty Acids in Korean Margarine)

  • 조영자;관야도광
    • 한국식품과학회지
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    • 제17권3호
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    • pp.219-222
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    • 1985
  • 한국산 가정용 마아가린을 1983년과 1984년 및 대만산을 각기 11종, 19종과 4종을 시정에서 구입하여 GLC로 분석하였다. 1983년 제품은 trans-octadenoic arid가 $6.2{\sim}35.5%$(평균 18%)이었고 t,t-octadecadienoic acid는 없었다. 트란스-지방산은 linoleic acid함량이 증가할수록 감소하였다. 1984년도의 마아가린은 1983년 제품에 비하여 트란스지방산 함량이 감소하는 대신에 linoleic acid는 증가하였다. P/S ratio는 1984년도의 연질형(軟質型)에서 증가를 나타냈다. 한국산 마아가린은 일본산 마아가린보다 linoleic acid함량이 다소 작게 나타났다.

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Isolation and Characterization of Antioxidative Compounds from the Aerial Parts of Angelica keiskei

  • Kim, So-Joong;Cho, Jeong-Yong;Wee, Ji-Hyang;Jang, Mi-Young;Kim, Cheol;Rim, Yo-Sup;Shin, Soo-Cheol;Ma, Seung-Jin;Moon, Jae-Hak;Park, Keun-Hyung
    • Food Science and Biotechnology
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    • 제14권1호
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    • pp.58-63
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    • 2005
  • Ethyl acetate-soluble neutral fraction of hot water extracts from the aerial parts of Angelica keiskei showed a 1, 1-diphenyl-2-picrylhydrazyl (DPPH) radical-scavenging activity. Six antioxidative compounds were purified and isolated by various chromatographic procedures. Based on the analyses of FAB-MS and NMR, the isolated compounds were structurally elucidated as luteolin 7-O-${\beta}$-D-glucopyranoside (1), quercetin 3-O-${\beta}$-D-galactopyranoside (2), quercetin 3-O-${\beta}$-D-glucopyranoside (3), quercetin 3-O-${\alpha}$-D-arabinopyranoside (4), kaempferol 3-O-${\alpha}$-D-arabinopyranoside (5), and luteolin 7-O-rutinoside (6). The glycosides of flavonols and luteolin showed DPPH radical-scavenging activity. One molecule of 2, 3, 4, 6, 1, and 5 scavenged 4.2, 4.2, 4.1, 2.5, 2.2, and 1.4 molecules of DPPH radical, respectively.

식용 돼지췌장 리파제가 저급지방산 생성과 체다치즈 풍미향상에 미치는 영향 (Effects of Food Grade Porcine Pancreatic Lipase on the Production of Short-Chain Fatty Acids and its Contribution)

  • 곽해수;전익준;박정남
    • 한국식품과학회지
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    • 제22권3호
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    • pp.248-254
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    • 1990
  • 식용 돼지췌장 리파제를 두 가지 함량으로 치즈제조시 혼합하여 $7^{\circ},\;13^{\circ},\;21^{\circ}C$에서 숙성시켰다. GC 분석결과 효소처리한 치즈에서는 Control에서 보다 훨씬 많은 양의 저급지방산이 생성되었다. 돼지췌장 리파제를 많이 넣어 $21^{\circ}C$에서 숙성시킨 치즈의 경우 1주 후에 medium flavor 치즈, 3주 후에 거의 sharp flavor 치즈가 특별한 결함없이 생산되었다. 또한 이 효소를 조금 넣은 치즈에서는 양호한 질의 치즈가 많았는데, $7^{\circ},\;13^{\circ},\;21^{\circ}C$에서 3주부터 15주의 숙성기간 중 medium과 sharp flavor 치즈가 생산되었다. 통계분석에 의하면 체다풍미와 caproic acid의 함량에서, 또 체다풍미와 butyric acid, caproic acid 혼합함량 상호관계에서 유의성이 있었다. 적합한 조건을 사용한다면 돼지췌장 리파제는 체다치즈의 숙성을 촉진시키는데 사용 가능한 것으로 사료된다.

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A Curcuminoid and Two Sesquiterpenoids from Curcuma zedoaria as Inhibitors of Nitric Oxide Synthesis in Activated Macrophages

  • Jang, Mi-Kyung;Lee, Hwa-Jin;Kim, Ji-Sun;Ryu , Jae-Ha
    • Archives of Pharmacal Research
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    • 제27권12호
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    • pp.1220-1225
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    • 2004
  • The overproduction of nitric oxide (NO) by inducible nitric oxide synthase (iNOS) is known to be responsible for vasodilation and hypotension observed in septic shock and inflammation. Inhibitors of iNOS, thus, may be useful candidates for the treatment of inflammatory diseases accompanied by overproduction of NO. In the course of screening oriental anti-inflammatory herbs for the inhibitory activity of NO synthesis, a crude methanolic extract of Curcuma zedoaria exhibited significant activity. The activity-guided fractionation and repetitive chromatographic procedures with the EtOAc soluble fraction allowed us to isolate three active compounds. They were identified as 1,7-bis (4-hydroxyphenyl)-1,4,6-heptatrien-3-one (1), procurcumenol (2) and epiprocurcumenol (3) by spectral data analyses. Their concentrations for the 50% inhibition of NO production $(IC_{50})$ in lipopolysaccharide (LPS)-activated macrophages were 8, 75, 77 ${\mu}M$, respectively. Compound 1 showed the most potent inhibitory activity for NO production in LPS-activated macrophages, while the epimeric isomers, compound 2 and 3 showed weak and similar potency. Inhibition of NO synthesis by compound 1 was very weak when activated macrophages were treated with 1 after iNOS induction. In the immunoblot analysis, compound 1 suppressed the expression of iNOS in a dose-dependent manner. In summary, 1,7-bis (4-hydroxyphenyl)-1,4,6-heptatrien-3-one from Curcuma zedoaria inhibited NO production in LPS-activated macrophages through suppression of iNOS expression. These results imply that the traditional use of C. zedoaria rhizome as anti-inflammatory drug may be explained at least in part, by inhibition of NO production.

Investigation of Degradation Mechanism of Rabeprazole with Solid State Pharmaceutical Excipients

  • Ren, Shan;Tran, Thao Truong-Dinh;Tran, Phuong Ha-Lien;Rhee, Yun-Seok;Lee, Beom-Jin
    • Journal of Pharmaceutical Investigation
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    • 제40권6호
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    • pp.367-372
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    • 2010
  • Rabeprazole sodium (RPN) is known to be very unstable at acidic condition or some acidic pharmaceutical excipients such as acrylic acid polymer (carbomer 934) with carboxylic acids. Thus, degradation mechanism of binary blends of rabeprazole with pharmaceutical excipients in a solid state without using solvents at three different ratios (3:1, 1:1 and 1:3) was investigated using Fourier transform infrad (FTIR) spectroscopy. Alkalizer (MgO), neutral hydroxypropymethylcellulose (HPMC 4000) were also tested for comparison. The binary blends were stored under accelerated conditions ($40^{\circ}C$/75% relative humidity) for two weeks. The concentration of thioether rabeprazole from the binary blends with acidic carbomer 934 increased as the rabeprazole concentration decreased. In addition, the degradation half-life of rabeprazole as well as the relative peak area ratios obtained from FTIR spectra of S=O stretching at $1094.1\;cm^{-1}$ decreased consistently as the fraction of carbomer 934 increased due to its sensitivity between the basic benzimidazole nitrogen and carboxylic acid group of carbomer 934. The physical appearance also turned into strong brown color in the presence of carbomer 934. In contrast, there were no significant changes in the degradation kinetics of rabeprazole with MgO and HPMC 4000 in a solid state. This present study demonstrated that the solid-state compatibility test with the aid of HPLC chromatographic and FTIR spectral analyses could offer a valuable methodology to select suitable pharmaceutical excipients and to elucidate the degradation mechanism of RPN for drug formulations at the early formulation stages.

New dammarane-type triterpenoid saponins from Panax notoginseng saponins

  • Li, Qian;Yuan, Mingrui;Li, Xiaohui;Li, Jinyu;Xu, Ming;Wei, Di;Wu, Desong;Wan, Jinfu;Mei, Shuangxi;Cui, Tao;Wang, Jingkun;Zhu, Zhaoyun
    • Journal of Ginseng Research
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    • 제44권5호
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    • pp.673-679
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    • 2020
  • Background: Panax notoginseng saponin (PNS) is the extraction from the roots and rhizomes of Panax notoginseng (Burk.) F. H. Chen. PNS is the main bioactive component of Xuesaitong, Xueshuantong, and other Chinese patent medicines, which are all bestselling prescriptions in China to treat cardiocerebrovascular diseases. Notoginsenoside R1 and ginsenoside Rg1, Rd, Re, and Rb1 are the principal effective constituents of PNS, but a systematic research on the rare saponin compositions has not been conducted. Objective: The objective of this study was to conduct a systematic chemical study on PNS and establish the HPLC fingerprint of PNS to provide scientific evidence in quality control. In addition, the cytotoxicity of the new compounds was tested. Methods: Pure saponins from PNS were isolated by means of many chromatographic methods, and their structures were determined by extensive analyses of NMR and HR-ESI-MS studies. The fingerprint was established by HPLC-UV method. The cytotoxicity of the compounds was tested by 3-(4,5-dimethylthiazol-2-yl)-2,5 -diphenyltetrazolium bromide assay. Results and Conclusion: Three new triterpenoid saponins (1-3) together with 25 known rare saponins (4-28) were isolated from PNS, except for the five main compounds (notoginsenoside R1 and ginsenoside Rg1, Rd, Re, and Rb1). In addition, the HPLC fingerprint of PNS was established, and the peaks of the isolated compounds were marked. The study of chemical constituents and fingerprint was useful for the quality control of PNS. The study on antitumor activities showed that new Compound 2 exhibited significant inhibitory activity against the tested cell lines.