• Archives of Pharmacal Research
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• 제29권1호
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• pp.46-49
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• 2006

In this study, 2-N-arylimino-2,3-dihydro-1,3,4-thiadiazoles derivatives (6a-h) were synthetized. The mechanism of the studied reactions was discussed. The chemical structures of the compounds were elucidated by their IR, $^1H-NMR,\;^{13}C-NMR$, and Mass spectral data and elemental analyses. The compounds were tested for antimicrobial activity using diffusion agar technique.

• Bulletin of the Korean Chemical Society
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• 제32권10호
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• pp.3644-3649
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• 2011

Multinuclear solid-state nuclear magnetic resonance (NMR) experiments were performed to investigate the local structure changes of nanoporous silica during hydrothermal treatment and surface modification with 3-aminopropyltriethoxysilane (3-APTES). The nanoporous silica was prepared by sol-gel polymerization using inexpensive sodium silicate as a silica precursor. Using $^1H$ magic angle spinning (MAS) NMR spectra, the hydroxyl groups, which play an important role in surface reactions, were probed. Various silicon sites such as $Q^2$, $Q^3$, $Q^4$, $T^2$, and $T^3$ were identified with $^{29}Si$ cross polarization (CP) MAS NMR spectra and quantified with $^{29}Si$ MAS NMR spectra. The results indicated that about 25% of the silica surface was modified. $^1H$ and $^{29}Si$ NMR data proved that the hydrothermal treatment induced dehydration and dehyroxylation. The $^{13}C$ CP MAS and $^1H$ MAS NMR spectra of 3-APTES attached on the surface of nanoporous silica revealed that the amines of the 3-aminopropyl groups were in the chemical state of ${NH_3}^+$ rather than $NH_2$.

• Bulletin of the Korean Chemical Society
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• 제30권5호
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• pp.1039-1042
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• 2009

RNA polymerase II C-terminal domain phosphatase 1 containing ubiquitin like domain (UBLCP1) has been identified as a regulatory molecule of RNA polymerase II. UBLCP1 consists of ubiquitin like domain (UBL) and phosphatase domain homologous with UDP and CTD phosphatase. UBLCP1 was cloned into the E.coli expression vectors, pET32a and pGEX 4T-1 with TEV protease cleavage site and purified using both affinity and gel-filtration chromatography. Domains of UBLCP1 protein were successfully purified as 7 mg/500 mL (UBLCP1, 36.78 KDa), 32 mg/500 mL (UBL, 9 KDa) and 8 mg/500 mL (phosphatase domain, 25 KDa) yielded in LB medium, respectively. Isotope-labeled samples including triple-labeled ($^2H/^{15}N/^{13}C$) UBLCP1 were also prepared for hetero-nuclear NMR experiments. $^{15}N-^{1}H$ 2D-HSQC spectra of UBLCP1 suggest that both UBL and phosphatase domain are properly folded and structurally independent each other. These data will promise us further structural investigation of UBLCP1 by NMR spectroscopy and/or X-ray crystallography.

• Natural Product Sciences
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• 제4권4호
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• pp.245-252
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• 1998

The unique sulphated phenolics, gallic acid 3-methyl ether 5-potassium sulphate, isoferulic acid 3-potassium sulphate, and ellagic acid 4,4'-dimethyl ether 3-potassium sulphate have been isolated from the flowers of Tamarix amplexicaulis Ehrenb. (Tamaricaceae). The hitherto unknown natural phenolic acid, gallic acid 3-methyl ether, together with the known phenolic, gallic acid, gallic acid 4-methyl ether, isoferulic acid, ferulic acid, ellagic acid, and ellagic acid 4,4'-dimethyl ether have been also separated and characterized. The structures were established by conventional methods, including electrophoretic analysis and confirmed by ESI-MS, $^1H-\;and\;^{13}C-NMR$.

• Applied Biological Chemistry
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• 제40권1호
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• pp.85-88
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• 1997

Chrysanthemum속(屬) 식물의 성분 및 생리활성물질에 대한 연구의 일환으로, 구절초 꽃의 chloroform 분획물을 재료로 B. subtilis, 및 V. aureus 및 v. parahaemolyticus에 대한 activity-guieded fractionation을 실시하여 항균성 물질 두가지를 얻었다. 항균력실험 결과,화합물I은 $100\;{\mu}g/disk$의 농도에서 세가지균주 모두에 활성이 있었고 화합물 II는 B. subtilis와 V. parahaemolyticus에만 활성이 나타났다. 화합물 I과 화합물 II는 현재 식품보존료로 사용되는 benzoic acid 및 sorbic acid와 비교해볼 때, B. subtilis와 v. perahaemolyticus에 대하여 대략 5배정도 강한 항균력을 나타내었다. $^1H,\;^{13}C\;NMR,\;DEPT,\;^1H-^1H\;COSY,^{13}C-^1H\;COSY$ 및 Mass spectrum 등을 분석한 결과, 화합물 I과 II는 sesquiterpene lactone인 angeloylcumambrin B($C_{20}H_{25}O_5,$ MW=346)와 cumambrin A($C_{17}H_{25}O_5,\;W=346$)로 각각 동정되었으며 이들은 구절초에서는 처음 분리되었다.

• Applied Biological Chemistry
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• 제46권2호
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• pp.69-73
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• 2003

병원에서 분리한 azole계 항진균성 항생물질에 대한 내성을 가지고 있는 Candida albicans에 대해 강한 활성을 가지는 항진균성 물질을 Bacillus subtilis LAM 97-44의 배양액으로부터 분리 정제한 후 그 특성을 조사하였다. 원심분리한 배양상등액을 butanol 추출, Diaion HP-20과 Dowex-50 adsorption chromatography, silica gel flash chromatography와 HPLC로 정제하였고 TLC와 HPLC로 확인하여 그 물질을 LAM-44A라 명명하였다. LAM-44A는 pH와 열에 매우 안정하였으며 Candida sp., Cryptococcus sp. 등에 대해 강한 활성을 나타낸 반면에 독성은 매우 적었다. 분리한 물질은 273 m에서 최대흡광도를 가진 융점 $202^{\circ}C$의 무색분말이었으며 ninhydrin 반응결과 음성이었고 $^1H-NMR$, $^{12}C-NMR$, IR spectrum, 원소분석 등의 결과로 볼 때 분자량 282의 $C_{14}H_{34}O_5$의 화학식을 가진 물질로 동정되었다.

• Journal of Microbiology and Biotechnology
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• 제16권10호
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• pp.1591-1596
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• 2006

Acaricidal effects of materials derived from Caesalpinia sappan heartwoods against Dermatophagoides farinae and D. pteronyssinus were assessed and compared with those evidenced by commercial benzyl benzoate and DEET. The observed responses varied according to dosage and mite species. The $LD_{50}$ values of the methanol extracts derived from C. sappan heartwoods were 6.13 and $5.44{\mu}g/cm^3$ against D. farinae and D. pteronyssinus, respectively. Furthermore, the ethyl acetate fraction derived from the methanol extract was approximately 8.71 more toxic than DEET against D. farinae, and 4.73 times more toxic against D. pteronyssinus. The biologically active constituent from the ethyl acetate fraction of C. sappan heartwood extract was purified via silica gel chromatography and high-performance liquid chromatography. The structure of the acaricidal component was analyzed by $GC-MS,\;^1H-NMR,\;^{13}C-NMR,\;^1H-^{13}C\;COSY-NMR$, and DEPT-NMR spectroscopy, and identified as juglone (5-hydroxy-l,4-naphthoquinone). Based on the $LD_{50}$ values of juglone and its derivatives, the most toxic compound against D. farinae was juglone ($0.076{\mu}g/cm^3$), followed by benzyl benzoate ($9.143{\mu}g/cm^3$) and 2methyl-l,4-naphthoquinone ($40.0{\mu}g/cm^3$). These results indicate that the acaricidal activity of C. sappan heartwoods is likely to be the result of the effects of juglone. Additionally, juglone treatment was shown to effect a change in the color of the cuticles of house dust mites, from colorless-transparent to dark brownish-black. Accordingly, as a naturally occurring acaricidal agent, C. sappan heartwood-derived juglone should prove to be quite 'useful as a potential control agent, lead compound, and house dust mite indicator.

• Applied Biological Chemistry
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• 제46권3호
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• pp.246-250
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• 2003

양하(Zingiber mioga Roscoe) 근경의 에탄을 추출물을 재료로 Staphylococcus aureus, Bacillus subtilis 및 B. cereus에 대한 activity-guided fractionation을 실시하여 항균성 물질 세가지준 얻었다. 항균력실험 결과, 화합물 I과 111은 세가지균주 모두에 활성이 있었고, 화합물 II에서는 B. subtilis과 B. cereus에서만 활성이 나타났다. 그 중에서 가장 활성이 강한 화합물 I을 Bioscreen C로 optical density(600 nm)를 측정하여 증식억제실험을 한 결과 10 ppm 처리시 B. subtilis과 B. cereus에서 72시간동안 강한 증식억제효과를 나타내었으며, S. aureus에서는 25 ppm 처리시 72시간동안 완전증식억제효과를 나타내었다. $1^H-NMR$, ${13}^C-NMR$, DEPT,$1^H-1^H$ COSY, HMQC, HMBC 및 IR 스펙트럼 등을 분석한 결과 화합물 I, II, III은 labdane-type diterpene인 $(E)-8{\beta}(17)-epoxylabd-12-ene-15,16-dial(C_{20}H_{30}O_3,\;MW=318)$, $galanolactone(C_{20}H_{30}O_3,\;MW=318)$ 그리고 galanal A($C_{20}H_{30}O_3,\;MW=318$)로 각각 동정되었으며, 이들은 양하의 근경에서는 처음 분리된 것이다.

• 임산에너지
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• 제21권1호
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• pp.41-48
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• 2002

참나무속 상수리나무와 굴참나무 수피를 채취하여 아세톤-물(7:3, v/v) 혼합용액으로 추출하고 유기용매를 제거한 후 hexane, CH₂C1₂, EtOAc 및 수용성으로 분획하여 동결건조하였다. 두 수종의 EtOAc용성 분획물은 MeOH 수용액 및 EtOH-hexane 혼합용액을 사용하여 Sephadex LH-20 칼럼크로마토그래피를 수행하였다. 단리된 화합물의 구조는 ¹H, /sup 13/C 및 2D-NMR spectrum으로 구조를 구명하였다. 화합물의 분자량은 FAB-MS로 측정하였다. 굴참나무에서는 (+)-catechin, caffeic acid, taxifolin-3-O-β-D-glucopyranoside를 단리 하였으며 상수리나무에서는 (+)-catechin, (+)-gallocatechin, gallic acid, taxifolin-3-O-β-D-glucopyranoside를 단리 하였다.

• 한국식품저장유통학회지
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• 제15권6호
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• pp.878-883
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• 2008

항균력이 탁월한 매실추출물로부터 항균활성물질을 column chromatography를 이용하여 순수하게 분리하고, nuclear magnetic resonance (NMR) spectrophtometer 측정기에 의하여 항균활성물질의 화학구조를 다음과 같이 분리 동정하였다. 즉, 매실추출물을 상온에서 메탄올에 현탁한 후, ethyl ether, ethyl acetate, n-butanol로 각각 분배 추출하여 각 용매의 수용성 추출물을 획득하였다. 각 용매의 수용성 추출물을 loading한 후, silica gel(70-230 mesh, Merck) column chromatography하여 소획분을 얻었다. 분리된 분획 중 항균력이 있는 소획분을 Sephadex LH 20을 충진하고 column chromatography하여 각 항균분획물질을 분리하였다. column chromatography에서 분리한 각 항균분획물질(Compound A, Compound B, Compound C)의 구조분석을 위해 $^{1}H$ 및 $^{13}C$ NMR 스펙트럼을 실온에서 측정하였다. NMR은 Bruker DRX500 (500MHz)을 이용하여 측정하였으며, 용매와 기준물질은 $CDCl_3$와 TMS를 각각 사용하였다. 이와같이 분리한 각 항균분획물질을 NMR 분석법으로 동정한 결과, isoeugenol, nomilin 및 $\beta$-sitosterol 등으로 확인되었다.